Food Analytical Methods

, Volume 10, Issue 6, pp 1709–1720 | Cite as

Authenticity Assessment of the “Onisiówka” Nalewka Liqueurs Using Two-Dimensional Gas Chromatography and Sensory Evaluation

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Abstract

The “Onisiówka” nalewka liqueur is a regional Polish alcoholic beverage, which is inscribed on the list of regional and traditional products of the Ministry of Agriculture and Rural Development in Poland. It is produced from multiflower honey, black elderberry flower syrup, and spirit. Due to fact that the “Onisiówka” nalewka liqueur has never been investigated, these studies are the foundation for further work on this regional alcoholic beverage. The main aim of this work is the authenticity assessment of the “Onisiówka” nalewka liqueurs by means of qualitative characteristics of volatile fraction and sensory evaluation. Tentative identification has been performed using two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). Application of GC×GC-TOFMS allowed for detection of around 350 compounds present in the volatile fraction of the “Onisiówka” from which 102 compounds were tentatively identified. PCA results showed that the first two principal components constitute 96.98% of total variance. Statistical analysis was used to visualize relations between tentatively identified compounds; therefore, it has been demonstrated that 23 chemical compounds may have significant influence on the overall flavor and taste of the “Onisiówka”. These substances belong to four chemical classes, in which the greatest number is represented by esters (13), aldehydes (6), alcohols (3), and one terpene compound. According to the sensory evaluation, the Onisiówka is characterized by sweet, honey, fruity, flowery, bitter, and spirituous flavor and taste.

Keywords

Onisiówka Nalewka Liqueur GC×GC-TOFMS Sensory evaluation Authenticity test 

Introduction

Liqueurs constitute important group of spirit beverages on the global market, which are representing a wide range of traditional drinks (Christoph and Bauer-Christoph 2006). According to the Regulation of the European Union, they are spirit drinks produced by flavoring ethyl alcohol or distillate of agricultural origin by foodstuff such as fruit, herbs, wine, or other agricultural products and sweetened (Regulation [EC] No. 110/2008). The minimum content of alcohol is 15% v/v, and most frequently, liqueurs are colored by adding agricultural food products, such as caramel and honey. The most popular liqueurs are made of cherries, citrus, herbs, apples, and blackcurrants (Christoph and Bauer-Christoph 2006; Śliwińska et al. 2015). Generally, these beverages are used as aperitif and are served in small glasses after the meal (Egea et al. 2015).

In the scientific literature, there are information about the analysis of liqueurs made from cherry (Ieri et al. 2012; Śliwińska et al. 2016a; Senica et al. 2016), apple (Śliwińska et al. 2016b), lemon (Schipilliti et al. 2013; Naviglio et al. 2015; Naviglio et al. 2016), melon (Hernández Gómez et al. 2009), pineapple (Oliveira et al. 2015), herb (Vázquez-Araújo et al. 2013), and walnut (Stampar et al. 2006; Jakopic et al. 2007). Most studies of these beverages are conducted using chromatography, sensory evaluation, and recently electronic sensing. Among all chromatographic techniques most often used for identifying volatile fraction of alcoholic beverages is one-dimensional gas chromatography (GC) (Śliwińska et al. 2015). Despite the fact that relatively long time GC analysis allows for separation of around several hundred substances in single run, one-dimensional retention mechanism usually is not enough to prevent co-elution phenomena (Welke and Alcaraz Zini 2011; Cordero et al. 2015). Therefore, more and more often, two-dimensional gas chromatography (GC×GC) is used to analyze alcoholic beverages. The GC×GC-time-of-flight mass spectrometry (TOFMS) technique has found application in wine (Weldegergis et al. 2011; Welke et al. 2012; Samykanno et al. 2013; Bordiga et al. 2013), cachaça (Cardeal et al. 2008; Cardeal and Marriott 2009; Capobiango et al. 2013), and selected spirit beverages (such as vodka, whisky, tequila) (Cardeal and Marriott 2009), also fruit spirit (Villière et al. 2012; Capobiango 2015), Japanese sake (Takahashi et al. 2016), and Chinese liqueur (Zhu et al. 2007; Yao et al. 2015) analysis.

The variety of liqueurs depends primarily on the geographical origin and climatic conditions of the region in which they are produced. Consequently, this affects the choice of ingredients for the production of liqueurs. In order to protect the traditional and specific for a particular region food products, they are labeled as “Protected Destination of Origin” (PDO), “Protected Geographical Indication” (PGI), and “Traditional Specialty Guaranteed” (TSG), all in accordance with guidelines of the European Union (Śliwińska et al. 2016c). To the group of geographical indications of liqueurs by EU belong, among others, Liquore di limone di Sorrento (Italy), Licor de hierbas de Galicia (Spain), Ratafia de Champagne (France), and Berliner Kümmel (Germany) [Regulation [EC] No. 110/2008; EU Agricultural Product Quality Policy]. Year after year, the list of traditional products designated by the EU is growing. Consequently, analytical techniques are used for authenticity tests, quality control, and adulteration assessment of foodstuff (Borràs et al. 2015). For this reason, the GC×GC-TOFMS instrument is increasingly applied in analysis of regional food products certified by EU commission in terms of profiling, fingerprinting, and traceability of origin. This approach has already been included in studies that concerned hazelnuts (Tonda gentile romana) (Cordero et al. 2008), honeys (Corsican honey) (Cajka et al. 2009; Stanimirova et al. 2010), and olive oils (Monti Iblei, Dauno Gargano) (Magagna et al. 2016).

One of the traditional Polish alcoholic beverages unspecified by the EU is the “Onisiówka” nalewka liqueur. However, this drink, since 2006, was inscribed on the list of regional and traditional products of the Ministry of Agriculture and Rural Development in Poland (Traditional Polish Products). Food products located on this list are of high quality and originate from specific regions and characterize by the traditional method of their production dating back at least 25 years (Journal of Laws No. 10/2005, item 68). The “Onisiówka” nalewka liqueur is manufactured according to familial recipe, almost 40 years of tradition. The origin of this beverage is closely connected with the farmhouse “Pasieka Wędrowna Barć” located in the village Krzemienica in Pomeranian Voivodeship. Precisely from this region come all the ingredients needed to prepare the “Onisiówka” nalewka liqueur such as multiflower honey, black elderberry flower syrup called “hyczka”, and spirit. All components are combined without any processing (heating, distillation) in order not to destroy the natural flavors of all ingredients (“Wędrowna Barć”). The final content of alcohol is around 40% v/v (Traditional Polish Products). According to Śliwińska et al. (2016a), this beverage may be labeled nalewka, because it is prepared exclusively in homemade conditions. In addition, the main ingredient of this beverage is honey; therefore, the “Onisiówka” nalewka liqueur should not be confused with mead, which is produced by yeast alcoholic fermentation of diluted honey (Pereira et al. 2014, 2015; Dobrowolska-Iwanek 2015).

It is possible to find information about the analysis of volatile fraction of the main ingredients of the “Onisiówka” such as honey (Pontes et al. 2007; Rivellino et al. 2013), black elderberry fruits (Ochmian et al. 2010; Vítová et al. 2015), and flowers (Kaack and Christensen 2008). However, the “Onisiówka” nalewka liqueurs have never been investigated. For that reason, knowledge about this regional and traditional beverage should be increased. The main aim of this work is the authenticity assessment of the Onisiówka nalewka liqueurs by means of qualitative characteristics of volatile fraction and sensory evaluation. Tentative identification has been performed by GC×GC-TOFMS, and statistical analysis was made using Principal Component Analysis (PCA).

Materials and Methods

Samples, Chemicals, and Materials

Five bottles of the “Onisiówka” nalewka liqueurs were acquired from original producer, Agroturism Farm “Pasieka Wędrowna Barć” (Krzemienica, Poland) in Pomeranian Voivodeship in 2014. Figure 1 presents original bottle and label of this beverage. Tightly sealed and secured bottles of beverages were stored in below room temperature in the dark place prior to analysis.
Fig. 1

Original bottle of 250 ml and label of “Onisiówka” nalewka liqueur

A C7–C30 alkane mixture for linear retention index (linear temperature programmed retention index (LTPRI)) calculations was from Sigma-Aldrich (St. Louis, MO, USA).

Sample Preparation

Samples for GC×GC-TOFMS analysis were prepared in the proportion of 2 ml of liqueur “Onisiówka” and 4 ml of deionized water and then transferred into 20-ml glass vials (Śliwińska et al. 2016d). All samples were sealed with magnetic screw caps closing with 1.3-mm-thick PTFE/silicone septum purchased from Sigma-Aldrich (Poznań, Poland). High-purity deionized water used for diluting liqueurs was obtained from a MilliQ A10 Gradient/Elix System (Millipore, USA). During the research ten repetitions were performed for each sample.

Samples for sensory evaluation contained 20 ml of “Onisiówka” nalewka liqueur.

Headspace Generation

The headspace generation for GC×GC-TOFMS procedure was preceded by headspace solid-phase microextraction (HS-SPME) extraction. A Gerstel autosampler (MPS autosampler, Gerstel, Mülheim, Germany) with agitator and SPME fiber conditioning station was used to extract the volatile compounds from liqueurs. The SPME fiber with divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS, thickness of 50/30 μm, length of 1 cm) coating (Sigma-Aldrich, Munich, Germany) was used. Prior to GC×GC-TOFMS analysis, the fiber was conditioned according to the instructions provided by the producer. Before the extraction, the samples were kept at 40 °C for 5 min. During the extraction, the vial was agitated at 700 rpm. Extraction was carried out at 40 °C for 20 min. After the extraction, the fiber was removed from the vial and transferred to the injector of a gas chromatograph for thermal desorption of the analytes at 250 °C for 5 min (Śliwińska et al. 2016a).

Instrumentation

The GC×GC system consisting of an Agilent 7890A equipped with liquid nitrogen-based quad-jet cryogenic modulator and a split/splitless injector, and Pegasus 4D TOFMS (LECO Corp., St. Joseph, MI, USA) was used for analysis. The first dimensional nonpolar column was 30 m × 0.25 mm i.d. × 0.25 μm film thickness Equity-1 (Supelco, Bellefonte, PA, USA). The second dimensional polar column was 2 m × 0.1 mm i.d. × 0.1 μm film thickness SolGel-Wax (SGE Analytical Science, Austin, TX, USA).

The injector, transfer line, and ion source temperature was set at 250 °C. The separation was performed using the following temperature program for the primary oven: initial temperature 40 °C, kept for 3.5 min, ramped at 7 °C/min to 250 °C, and held for 5 min. The secondary oven temperature was programmed from 45 °C, kept for 3.5 min, ramped at 7 °C/min to 255 °C, and held for 2 min (Śliwińska et al. 2016a). The modulation period was 6 s. Hydrogen (N6.0 class) was used as a carrier gas at a flow rate at 1.0 ml/min. The transfer line was at 250 °C, and the ion source set was 250 °C. The detector voltage was 1600 V. Mass spectra were collected from m/z 40–400 at ten spectra per second. The acquisition delay was 460 s.

Sensory Evaluation

The sensory evaluation of the “Onisiówka” nalewka liqueur was performed using the point method (PN-64/A-04022). The number of ten panelists, comprising five women and five men, evaluated the flavor, taste, and color of each beverage according to a five-point scale (1—bad to 5—very good). All persons were selected to preliminary test of taste and small according to procedure (PN-A-79529-2:2005). Additionally, panelists were asked to describe the color and the most perceptible flavors and tastes. The panel tasting took place in an air-conditioned room (21 °C). The “Onisiówka” nalewka liqueur samples were evaluated in triple repetitions.

Data Processing

Analysis of the data obtained by the use of the GC×GC-TOFMS system was done using the algorithm for peak deconvolution with a baseline offset of 0.5 and signal to noise (S/N) set up at 100. The ChromaTOF software (LECO Corp., version 4.24) was used for this purpose. Tentative identification of volatile compounds in the “Onisiówka” nalewka liqueurs was obtained by comparing experimental LTPRIs with literature retention indices for first dimension GC (Welke et al. 2014a). Retention data of a series of n-alkane mixture, under the same experimental conditions, employed for the chromatographic analysis of beverage volatile fraction used for experimental LTPRI. These LTPRI values were calculated using Van den Dool and Kratz equation (Van Den Dool and Kratz 1963). Literature LTPRI values were obtained for 100% dimethyl polysiloxane capilary GC columns. Mass spectrometric information of each chromatographic peak was compared with NIST 2011 library considering with minimum similarity value of 85%. Whenever a LTPRI was not found in the scientific literature to match with the experimentally determined LTPRI or chemical compounds contain less than six carbon atoms, only then manual assess, with respect to the mass spectra match and the unique mass, was used for quantification.

Statistical Analysis

Statistical analysis was performed using GC×GC-TOFMS dataset consisting average values of peak areas, heights, and S/N ratio of 102 chemical compounds (taken from the ChromaTOF software), and data achieved after sensory evaluation consisting of all points of sensory assessment obtained by panelist group.

The statistical analysis was performed by using The Unscrambler v9.7 (CAMO Software AS, Oslo, Norway). A nonsupervised multivariate method, the PCA was used for visualization of relations between tentative identified compounds in the “Onisiówka” nalewka liqueur obtained using GC×GC-TOFMS. Results obtained from sensory evaluation were analyzed by using Microsoft Excel 2007 software. All figures were performed by using OriginPro 8.3 software (Northampton, MA, USA).

Results and Discussion

GC×GC-TOFMS Analysis

More than 350 compounds detected in each sample of the “Onisiówka” nalewka liqueur by GC×GC-TOFMS; 102 were tentatively identified with the following criteria: time of first dimension (1D) was set at 650 s, which was calculated on the basis of alkane mixtures, minimum of mass spectral similarity value set at 85%, S/N ratio set at 100, and the comparison of experimental and literature LTPRIs. Figure 2 shows a color plot obtained after HS-SPME/GC×GC-TOFMS analysis of the “Onisiówka” nalewka liqueur.
Fig. 2

Separation of volatiles of the “Onisiówka” nalewka liqueur isolated by the use of HS-SPME technique. Presented color plot of GC×GC-TOFMS chromatogram was made in mode of total ion mode current (TIC)

The threshold value of similarity parameter was established at 850 (which means the 85% similarity of experimental mass spectrum with the mass spectrum taken from the database of NIST 2011). Values below mentioned threshold and signal-to-noise ratio were not taken into consideration during further data analysis. Regarding Fig. 3, the identification method of chemical compound, for example, nonanal, based on database of mass spectrum, was explained.
Fig. 3

The example of tentatively identified nonanal extracted by the use of HS-SPME from the “Onisiówka” nalewka liqueur and analyzed through the GC×GC-TOFMS system. Identification was done on the basis of comparison of experimental data with the mass spectrum included in the database of NIST 2011. a, b Enlarged fragment of the region of color plot (3D) obtained using m/z = 57. c Experimental mass spectra of the compound and the respective mass spectra of the same substance included in NIST 2011 library

The number of chromatographic peaks found resulted by S/N ratio established in this study (over 100). LTPRI experimental values were calculated according to the Van den Dool and Kratz equation (Van Den Dool and Kratz 1963). Additionally, values of LTPRI for compounds containing six atoms of carbon (C6) were extrapolated. The values of LTPRI were also compared with literature LTPRI for every compound. The acceptance criteria were less than 15 units of difference between experimental and literature LTPRI. Due to these requirements, 102 volatile compounds were tentatively identified in the Onisiówka nalewka liqueurs (Table 1).
Table 1

The identification of compounds from the volatile fraction of the “Onisiówka” nalewka liqueur using HS-SPME/GC×GC-TOFMS

Name

Chemical formula

S.

U. mass

LTPRIExp

LTPRILit

Sensory description

I. n.

Alcohols

3-Methylbutanola

C5H12O

910.8

55

Alcoholic, balsamic, bitter, burnt, cheese, fermented, fruity

1

1-Hexanolb

C6H14O

926.7

56

850f

847.9

Floral, fruity, green, herbaceous, sweet

90

3-Hexen-1-olb

C6H12O

931.4

67

842.3

837

Fresh, green

9

1-Heptanol

C7H10O

915.2

70

960

951.8

Fresh, light green, nutty

13

Benzyl alcohol

C7H8O

907.6

79

1020

1022

Aromatic, floral, fruity, sweet

15

2-Phenylethanol

C8H10O

958.6

91

1092

1084

Floral, honey, lilac, rose, spice

92

1-Octen-3-ol

C8H16O

840.2

57

972

965

Carrot, herbaceous, spicy

20

2-Ethylhexanol

C8H18O

930.2

57

1020

1013

Citrus, green, rose,

25

1-Octanol

C8H18O

944.6

56

1056

1057

Fatty, floral, green, herbaceous

30

1-Nonanol

C9H20O

892.4

56

1144

1151

Fatty, floral, fruity, green

42

1-Dodecanol

C12H26O

942.8

69

1450

1457.1

Fatty, waxy

74

Aldehydes

2-Furancarboxaldehyde (furfural)a

C5H4O2

945.8

95

Almond, bread, sweet

8

2-Methyl-2-butenala

C5H8O

917.6

84

Cacao, coffee

3

Hexanalb

C6H12O

942.6

57

780.8

777

Acorn, fruity, grassy, herbaceous, leafy

5

Benzaldehyde

C7H6O

974

106

944

935

Almond, burnt sugar, fruity, woody

12

2-Hydroxybenzaldehyde

C7H6O2

921.8

122

1024

1024

Medicinal

16

Octanal

C8H16O

937.2

57

988

984

Citrus, fatty, floral, fruity

22

Benzeneacetaldehyde

C8H8O

955.2

91

1020

1010

Floral, grassy, green, rose, sweet

26

3-Octenal

C8H14O

900.6

70

1040

1031

Nf

27

2-Methylbenzaldehyde

C8H8O

931.4

91

1048

1038

Nf

29

3-Methylbenzaldehyde

C8H8O

931.4

91

1048

1057

Nf

93

4-Methylbenzaldehyde

C8H8O

882.8

91

1060

1064

Floral, fruity, mild, spicy, sweet

32

4-Methoxybenzaldehyde

C8H8O2

931

135

1204

1211

Anise, minty, sweet

36

Nonanal

C9H18O

945.6

57

1084

1083

Citrus, floral, fruity, lavender, melon

39

2-Phenylpropenal

C9H8O

928.4

103

1131

1150

Nf

40

4-Ethylbenzaldehyde

C9H10O

876.4

134

1148

Nf

Nf

43

2,4-Nonadienal

C9H14O

849.4

81

1176

1165

Watermelon

45

Decanal

C10H20O

959.8

57

1187

1184

Burnt, fatty, floral, green, lemon, orange peel

61

2-Decenal

C10H18O

912.2

70

1234.8

1237

Fatty, orange

63

2,4-Decadienal

C10H16O

860.4

81

1282.6

1290

Fatty

64

Dodecanal

C12H24O

951.6

57

1390

1385

Citrus, fatty, herbaceous, lily, oily, waxy

76

Butylphenyl methylpropional

C14H20O

850.6

189

1511.1

1500

Floral

80

Ketones

(E)-3-Penten-2-onea

C5H8O

928.8

69

Fruity

2

2-Heptanone

C7H14O

893.6

58

876

864

Cheese, fruity, nutty

10

6-Methyl-5-hepten-2-one

C8H14O

903

43

972

973

Blackcurrant, boiled fruit, citrus, pepper, woody

19

Acetophenone

C8H8O

966.2

105

1044

1043

Almond, cheese, floral, musty, sweet

28

2-Nonanone

C9H18O

885.2

58

1072

1073

Baked, fatty, fruity, green

37

4-Methylacetophenone

C9H10O

931.2

119

1152

1157

Almond, floral, hay, sweet

44

2-Decanone

C10H20O

924.6

58

1177.3

1175

Citrus, floral, orange

65

2-Undecanone

C11H22O

918

58

1272.7

1274

Fresh, fruity, green, musty, orange

67

2-Dodecanone

C12H24O

850.8

58

1375

1377

Citrus

77

2-Pentadecanone

C15H30O

878.2

58

1687.5

1688

Floral, herbaceous, spicy

84

Acids

Octanoic acid

C8H16O2

868.4

60

1160

1158

Cheese, fatty acid

35

Esters

Ethyl 2-hydroxypropanoatea

C5H10O3

925

45

Ethereal buttery, fruity

7

Ethyl 2-methylpropanoateb

C6H12O2

913.6

71

750

742

Nf

4

Butyl acetateb

C6H12O2

888.6

43

788.5

791

Banana, bitter, fruity, green, pear, pineapple, sweet

6

Ethyl pentanoate

C7H14O2

864.4

88

888

890

Fruity, grassy, green, minty, orange

11

Ethyl furoate

C7H8O3

913.2

95

1028

1029

Floral, plum

17

Ethyl hexanoate

C8H16O2

900.8

88

988

980

Anise, apple, fruity, strawberry, sweet

21

Hexyl acetate

C8H16O2

951.6

43

1000

987

Citrus, fruity, green, herbaceous, spicy

24

Ethyl diethoxyacetate

C8H16O4

850.6

47

1060

Nf

Nf

31

Methyl benzoate

C8H8O2

904.4

105

1071

1061.4

Floral, herbaceous, honey, watermelon, sweet

33

Diethyl butanedioate

C8H14O4

968.6

101

1136

1136

Floral, fruity, potato, watermelon

34

Ethyl heptanoate

C9H18O2

910

88

1080

1081

Fruity

38

Ethyl benzoate

C9H10O2

953.6

105

1140

1138.2

Camomile, fruity, minty, lavender, melon

41

Ethyl 2-hydroxybenzoate

C9H10O3

894.2

120

1128

1236.8

Floral, minty, sweet, wintergreen

46

Hexyl butanoate

C10H20O2

852.8

89

1179.9

1173

Apple, fruity, green

59

Ethyl octanoate

C10H20O2

929.6

88

1178.3

1173

Anise, floral, fresh, fruity, green, metholic, sweet

60

Ethyl benzeneacetate

C10H12O2

951.4

91

1213

1218

Anise, cinnamon, floral, fruity, sweet, waxy

62

Ethyl nonanoate

C11H22O2

911.6

88

1272.7

1279

Waxy

66

Ethyl 3-phenylpropionate

C11H14O2

911.2

104

1318.2

1320

Floral, pleasant, sweet

68

4-tert-Butylcyclohexyl acetate

C12H22O2

911.8

57

1360

1346

Balsamic

71

Ethyl decanoate

C12H24O2

931.8

88

1375

1379

Fruity, grape, waxy

72

2-Propenyl 3-cyclohexylpropanoate

C12H20O2

845.2

55

1405

1407

Fruity

73

Pentyl 2-hydroxybenzoate

C12H16O3

858

120

1540

1543

Nf

75

Ethyl undecanoate

C13H26O2

890.6

88

1473.7

1477

Nf

78

Hexyl salicylate

C13H18O3

914.2

120

1636.8

1652

Balsamic, floral, hay, herbaceous, waxy

79

Ethyl dodecanoate

C14H28O2

938.6

101

1572.2

1577

Leafy, mango, waxy

81

Benzyl benzoate

C14H12O2

895

105

1716.7

1726

Balsamic, herbaceous, oil

82

Ethyl tridecanoate

C15H30O2

896.6

88

1681.3

1677

Nf

83

Ethyl tetradecanoate

C16H32O2

935.4

101

1764.7

1778

Etheral, oily, waxy

85

Diisobutyl phthalate

C16H22O4

895.4

149

1811.8

1819

Nf

86

Isopropyl myristate

C17H34O2

887.2

60

1807.143

1827

Floral, oily fatty

87

Ethyl pentadecanoate

C17H34O2

939.6

88

1878.571

1877

Fruity, grassy, green, minty, orange, yeast

88

Ethyl hexadecanoate

C18H36O2

928.2

88

1978.571

1978

Mild sweet, waxy

89

Terpenes

α-Pinene

C10H16

863

93

939.1

932

Camphor, citrus, fruity, green, pine, woody

47

α-Myrcene

C10H16

914

93

986.9

983

Balsamic, fruity, lemon, spicy, sweet

48

Limonene

C10H16

938.4

68

1034.8

1025

Citrus, fruity, minty, orange, peely

49

1,8-Cineole

C10H18O

861.2

71

1034.8

1033

Camphor, herbaceous, mentholic, minty, sweet

50

(Z)-Linalool oxide (furan)

C10H18O2

926.6

59

1069.6

1070

Rose, wood

51

p-Cymene

C10H12

941.2

117

1086.9

1079

Balsamic, citrus, fruity, herbaceous, lemon, spicy

52

Terpinolene

C10H16

923.4

93

1091.3

1089

Fruity, herbaceous, pine, sweet, woody

53

Hotrienol

C10H16O

855.4

71

1095.5

1085

Fungal

95

Nerol oxide

C10H16O

919.2

68

1143.5

1144

Floral, green, oily, spicy

54

Terpinen-4-ol

C10H18O

858.8

93

1177.3

1172

Fruity, herbaceous, licorice, musty, spicy, sweet, terpenic, woody

96

α-Terpineol

C10H18O

897.8

59

1186.3

1183

Anise, floral, fruity, minty, oily, peach

97

Borneol

C10H18O

854.6

95

1165.2

1155

Balsamic, camphor, musty

56

(Z)-Rose oxide

C10H18O

892.6

139

1104.3

1093

Green

102

Menthol

C10H20O

942.6

71

1169.6

1173

Peppermint, mentholic

57

Gardenol

C10H12O2

865

104

1169.6

1165

Sweet

58

Neryl acetate

C12H20O2

864.6

93

1345

1343

Floral, fruity, raspberry, rose

98

Bornyl acetate

C12H20O2

890.6

93

1284

1276

Balsamic, camphor, herbaceous, pine

70

β-Damascenone

C13H18O

854

121

1378.9

1371

Apple, fruity, honey, sweet, tobacco

100

Others

Phenolb

C6HO

951

94

961.5

961

Medicinal, phenolic

101

Benzonitrile

C7H5N

910.8

103

960

956

Bitter almond, cherry

14

Toluene

C7H8

902.5

91

748

748

Caramelized, etheral, fruity, pungent

91

Benzofuran

C8H6O

905.6

118

988

968

Nf

23

1,2-Dimethylbenzene

C8H10

932.8

91

868

871

Futty, oily, pungent

18

2-Pentylfuran

C9H14O

851.3

81

984

980

Butter, fruity, green bean

94

1-Ethyl-3,5-dimethylbenzene

C10H14

866.4

119

1152.2

1050

Nf

55

Dodecane

C12H26

918.4

57

1205

1200

Alkane, fusel

69

1,1,6-Trimethyl-1,2-dihydronaphthalene (TDN)

C13H18O

851.3

157

1355.9

1336

Licorice

99

Similarity (S.): average of similarity of the mass spectrum of the “Onisiówka” volatile compounds with the spectra of standard compounds in NIST 2011. Unique mass (U. mass): the most unique ion selected using ChromaTOF data analysis software. Experimental linear temperature programmed retention index (LTPRI Exp ) calculated using alkane mixtures and nonpolar stationary phase (100% dimethyl polysiloxane). Literature LTPRI (LTPRI Lit ) on nonpolar stationary phase (100% dimethyl polysiloxane). Sensory description: the classification of olfactory sensation caused by certain chemical compound, which was described in (AroChemBase library). Identification number (I. n.): identification number of compound in PCA analysis. Not found (Nf): value of LTPRI and sensory description in the literature were not found. Identification of compound was based only on mass spectra from the NIST 2011

aCompounds contain less than C6. Identification was based only in mass spectra from the NIST 2011

bExtrapolated LTPRI for compounds with contain only C6 below the lower of alkane mixtures analyzed

Among 102 tentatively identified compounds present in the volatile fraction of the “Onisiówka” nalewka liqueurs by GC×GC-TOFMS, esters were present in highest numbers (32), followed by aldehydes (21), terpenes (18), ketones (10), alcohols (11), acid (1), and others (9), which includes alkanes (1), furans (2), nitriles (1), and aromatic hydrocarbons (5). Percentage distribution of chemical classes present in the volatile fraction of the “Onisiówka” nalewka liqueurs was shown in Fig. 4.
Fig. 4

Percentage contribution of chemical classes present in volatile fraction of the “Onisiówka” nalewka liqueur determined by the use of GC×GC-TOFMS

The greatest group by number of identified chemical compounds was esters. Esters were also characterized by the highest contribution in the volatile fraction of this beverage (Fig. 4). These compounds have major impact on the aroma profile of alcoholic beverages, and they influence flavor of final product. Generally, esters are mostly formed from estrification of fatty acids with alcohols during fermentation process (Christoph and Bauer-Christoph 2006). Ester content in alcoholic beverages is also affected by maceration process and sensory properties of ingredients such as fruits or herbs used for production. For this reason, a large amount of esters are identified in various alcohol beverages made from fruits, such as fruit spirits, wines, cognacs, and liqueurs (Nikićević et al. 2011; Welke et al. 2014b; Śliwińska et al. 2015). In general, esters of lower carboxylic acid and lower alcohols characterized with fruity sensory properties, for example, butyl acetate, ethyl pentanoate, ethyl hexanoate, hexyl acetate, ethyl 2-hydroxypropanoate, and ethyl octanoate. However, fatty acid esters like ethyl hexadecanoate contribute to waxy flavor (Jørgensen et al. 2000). Aldehydes, ketones, and alcohol are other large chemical groups of identified chemical compounds in the “Onisiówka”. According to Jørgensen et al. (2000) and Cajka et al. (2007) aldehydes, ketones, and alcohol represented major chemical groups of honey and elder flower volatile compounds. Most of them characterized fruity and floral flavor such as 3-methylbutanol, benzyl alcohol, 2-ethylhexanol, 1-octanol, 1-nonanol, hexanal, octanal, benzeneacetaldehyde, nonanal, 2-phenylpropenal, 2,4-nonadienal, decanal, 2-decenal, dodecanal, butylphenyl methylpropional, (E)-3-penten-2-one, 2-heptanone, 6-methyl-5-hepten-2-one, acetophenone, 2-nonanone, 4-methylacetophenone, 2-decanone, 2-undecanone, 2-dodecanone, and 2-pentadecanone. Most of these compounds were previously identified in several studies of honey, elderberry fruits, and flowers (Jørgensen et al. 2000; Baroni et al. 2006; Pontes et al. 2007; Kaack 2008; Kaack and Christensen 2008; Ochmian et al. 2010; Rivellino et al. 2013; Dymerski et al. 2013; Vítová et al. 2015). Benzaldehyde and benzenealdehyde have been reported as usual components of unifloral honey (Baroni et al. 2006). Also, benzaldehyde previously has been detected as the most abundant aromatic compound in headspace of elderberry flower drink (Jørgensen et al. 2000). Benzyl alcohol and 2-phenylethanol have been identified and described as contributors to the flavor of elderberry (Mikova et al. 1984). Terpenes are another chemical compound group, which have influence on sensory properties of fruit spirit beverages and liqueurs (Christoph and Bauer-Christoph 2006; Winterová et al. 2008). In this study, 18 terpenes were identified; most of them may affect the pleasant fruity and herbaceous flavor of the “Onisiówka”. Terpenes such as (Z)-rose oxide, nerol oxide, and hotrienol are responsible for the characteristic floral aroma of elder flowers (Farkas et al. 1995; Jørgensen et al. 2000). In addition, other identified terpenes such as α-terpineol, terpinen-4-ol, terpinolene, nerol oxide, (Z)-linalool oxide, limonene, and 1,8-cineole have been also detected previously in honeys, elderberry fruits, and flowers (Jørgensen et al. 2000; Jensen et al. 2001; Cajka et al. 2007). There are several compounds which have been reported as common compounds of various honeys, such as toluene, furan, furfural, and hotrienol (Pontes et al. 2007). In the literature, there is information that phenol was identified in different samples of honey (Dymerski et al. 2013). Compounds such as β-damascone, 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN), and 6-methyl-5-hepten-2-one have been also identified as contributor to elderberry flavors (Poll and Lewis 1986). Full sensory descriptions of all tentatively identified compounds in volatile fraction of the “Onisiówka” nalewka liqueur are, according to (AroChemBase library), described in Table 1. It may be noted that most of tentatively identified compounds originate from two main ingredients of this beverage: honey and elderberry flowers. It has been previously reported that honey and black elderberry flowers demonstrate antioxidant and health benefit properties (Malika et al. 2005; Thole et al. 2006; Charlebois 2007; Bertoncelj et al. 2007; Alzahrani et al. 2012; Sidor and Gramza-Michałowska 2015). It may be assumed that the “Onisiówka” nalewka liqueur has a positive impact on health.

In order to visualize the relations between tentative identified compounds (102) in the volatile fractions of the “Onisiówka” nalewka liqueurs, PCA analysis was performed (Fig. 5). For this statistical analysis, area, height, and signal-to-noise ratio of peak of each compound were used. PCA results showed that the first two principal components accounted for 96.98% of total variance. In II and III quarts, there are 79 compounds in the negative area of PC1. These compounds could not be separated; they are located in a large cluster. It means that the values of used variables are similar compared to all tentatively identified compounds present in the volatile fraction of the “Onisiówka” nalewka liqueurs. On the other hand, 23 compounds are located in I and IV quarts in the positive region of PC1. These compounds may be defined. Also, as observed in Fig. 5, these compounds are located in two groups. The first group is located between 0 and 500,000 value of PC1 (in Fig. 5, highlighted in blue color). This group includes the following compounds: octanal, ethyl benzoate, dodecanal, hexyl salicylate, 1-dodecanol, 4-tert-butylcyclohexyl acetate, limonene, ethyl benzeneacetate, butyl acetate, diethyl butanedioate, and ethyl hexanoate. The second group (in Fig. 5, highlighted in red color) is located in a wider range of PC1 from 500,000 to 3,600,000 and includes ethyl decanoate, ethyl nonanoate, 2-ethylhexanol, benzaldehyde, ethyl tetradecanoate, decanal, ethyl dodecanoate, 2-phenylethanol, ethyl hexadecanoate, 2-furancarboxaldehyde, ethyl octanoate, and nonanal. The PCA has shown that these groups of compounds may significantly influence the overall flavor and taste of the “Onisiówka”.
Fig. 5

PCA score plot corresponding to visualize the relations between tentative identified compounds of the “Onisiówka” nalewka liqueur using GC×GC-TOFMS

Sensory Evaluation

During sensory evaluation of the “Onisiówka” samples, panelist group evaluated color, flavor, and taste according to five-point scale, from 1 (bad) to 5 (very good). Results of this analysis were collected in Table 2. Additionally, panelists were asked to describe the color and the most perceptible flavors and tastes.
Table 2

Sensory assessment of the “Onisiówka” nalewka liqueurs according to five-point scale

Sensory assessment of the "Onisiówka"

Color

Flavor

Taste

2.75 ± 1.04

3.88 ± 0.64

3.88 ± 0.64

All given values were presented as arithmetic mean including standard deviation. Sensory evaluation carried out by the application of point method according to PN-64/A-04022

According to the panelist group, color assessment of the “Onisiówka” received average score of 2.75, and they described it like honey, lemon chiffon, or straw. In addition, each member of the panelist group observed that evaluated samples had sediment. That color assessment of the Onisiówka may be due to occurring of natural sediment in this beverage, which can detract from the visual appearance of the product (Cernivec 2013). However, according to the panelist group, the “Onisiówka” received higher scores for flavor and taste assessments. Most of them also showed that they sensed sweet, honey, fruity, flower, and bitterness flavor. These sensory properties of the “Onisiówka” originate from several tentatively indentified compounds inter alia 2-phenylethanol, decanal, ethyl octanoate, butyl acetate, ethyl hexanoate, and nonanal. It should be noted that the last mentioned compounds were presented in PCA (Fig. 5) score as chemical compounds characterized by the highest value of peak area, height, and signal-to-noise ratio. Probably, the bitterness of “Onisiówka” originated from used black elderberry flower syrup. All members of the panelist group noticed that spirituous flavor felt very intense. This is due to the use of spirit rather than vodka which has less alcohol content.

Conclusion

In this work, it has been reported for the first time the authenticity assessment of Polish regional beverage, the “Onisiówka” nalewka liqueurs, using qualitative characteristics of volatile fraction and sensory evaluation. The comprehensive approach has shown that GC×GC not only represents high separation power but also can further examine the complexity of investigated samples thanks both to the higher level of information achievable from the two-dimensional GC×GC separation and to the possibility of the use of reliable data for chemometric interpretation. This is also made possible by its high sensitivity, which extends identification prospects by taking into account minor components of samples. This study has emphasized advantages of a comprehensive and multidisciplinary approach to interpret the increased level of information that GC×GC separation can provide in selected purposes. Thus, the application of GC×GC-TOFMS has allowed for tentative identification of 102 chemical compounds from around 350 substances detected in volatile fraction of these beverages. Percentage contribution of chemical classes in volatile fraction is presented by esters (46.45%), aldehydes (31.48%), alcohols (11.61%), terpenes (6.52%), ketones (2.57%), one carboxylic acid (0.21%), and others (1.17%), which includes alkanes, furans, nitriles, and aromatic hydrocarbons. Multiflower honey, black elderflower syrup, and spirit are used for the production of the “Onisiówka” nalewka liqueur. Most of the tentatively identified chemical compounds originate from the abovementioned matrices. These molecular entities include benzaldehyde, octanal, 2-ethylhexanol, 2-phenylethanol, nonanal, 6-methyl-5-hepten-2-one, nerol oxide, and limonene. The majority of the tentative identified esters, aldehydes, alcohols, and ketones characterize fruity, floral, and green flavor of these beverages. Additionally, PCA statistical analysis was useful to visualize relations between the tentatively identified chemical compounds. The first two principal components constitute 96.98% of total variance, and it has demonstrated that 23 tentatively identified compounds may have significant influence on the overall flavor and taste of this liqueur. In sensory evaluation, the panelist group has assessed flavor and taste of this beverage as sweet, honey, fruity, flowery, bitter, and spirituous. The obtained results of sensory analysis are consistent with the fact of using certain ingredients utilized for production of this beverage. The natural sediment in the “Onisiówka” could be potentially an evidence confirming the use of natural products, such as honey and black elderflower syrup, in its production. The use of these ingredients may also be the reason of some medical properties of this liqueur. Due to the fact that the “Onisiówka” nalewka liqueurs have never been investigated, these studies are the foundation for further work on this regional alcoholic beverage. This research allows for dissemination of regional products and probably in the near future can constitute a supplementary material for documents concerning protection of this traditional product in compliance with guidelines of the European Union and apply for the list of the protection of geographical indications of spirit beverages.

Notes

Acknowledgements

Magdalena Śliwińska is thankful for “InnoDoktorant—Scholarships for PhD Students, Sixth Edition” for financial support and also the Agroturism Farm “Pasieka Wędrowna Barć” for supplying the “Onisiówka” nalewka liqueurs for analysis. The authors acknowledge the financial support for this study by Grant No. 2012/05/B/ST4/01984 from the National Science Centre of Poland.

Compliance with Ethical Standards

Conflict of Interest

Magdalena Śliwińska declares that she has no conflict of interest. Paulina Wiśniewska declares that she has no conflict of interest. Tomasz Dymerski declares that he has no conflict of interest. Waldemar Wardencki declares that he has no conflict of interest. Jacek Namieśnik declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

References

  1. Alzahrani HA, Boukraâ LA, Bellik Y, Abdellah F, Bakhotmah BA, Kolayli S, Sahin H (2012) Evaluation of the antioxidant activity of three varieties of honey from different botanical and geographical origins. Glob J Health Sci 4:191–196CrossRefGoogle Scholar
  2. AroChemBase library. AromaChemBase V4 software (Alpha M.O.S., Toulouse, France). Accessed 11 August 2016Google Scholar
  3. Baroni MV, Nores ML, Díaz Mdel P, Chiabrando GA, Fassano JP, Costa C, Wunderlin DA (2006) Determination of volatile organic compound patterns characteristic of five unifloral honey by solid-phase microextraction-gas chromatography-mass spectrometry coupled to chemometrics. J Agric Food Chem 54:7235–7241CrossRefGoogle Scholar
  4. Bertoncelj J, Doberšek U, Jamnik M, Golob T (2007) Evaluation of the phenolic content, antioxidant activity and colour of Slovenian honey. Food Chem 105:822–828CrossRefGoogle Scholar
  5. Bordiga M, Rinaldi M, Locatelli M, Piana G, Travaglia F, Coïsson JD, Arlorio M (2013) Characterization of Muscat wines aroma evolution using comprehensive gas chromatography followed by a post-analytic approach to 2D contour plots comparison. Food Chem 140:57–67CrossRefGoogle Scholar
  6. Borràs E, Ferré J, Boqué R, Mestres M, Aceña L, Busto O (2015) Data fusion methodologies for food and beverage authentication and quality assessment—a review. Anal Chim Acta 891:1–14CrossRefGoogle Scholar
  7. Cajka T, Hajslová J, Cochran J, Holadová K, Klimánková E (2007) Solid phase microextraction-comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the analysis of honey volatiles. J Sep Sci 30:534–546CrossRefGoogle Scholar
  8. Cajka T, Hajslova J, Pudil F, Riddellova K (2009) Traceability of honey origin based on volatiles pattern processing by artificial neural networks. J Chromatogr A 1216:1458–1462CrossRefGoogle Scholar
  9. Capobiango M, Oliveira ES, Cardeal ZL (2013) Evaluation of methods used for the analysis of volatile organic compounds of sugarcane (Cachaça) and fruit spirits. Food Anal Method 6:978–988CrossRefGoogle Scholar
  10. Capobiango M, Bittar Mastello R, Chin ST, de Souza OE, de Lourdes CZ, Marriott PJ (2015) Identification of aroma-active volatiles in banana Terra spirit using multidimensional gas chromatography with simultaneous mass spectrometry and olfactometry detection? J Chromatogr A 1388:227–235CrossRefGoogle Scholar
  11. Cardeal ZL, de Souza PP, da Silva MD, Marriott PJ (2008) Comprehensive two-dimensional gas chromatography for fingerprint pattern recognition in cachaça production. Talanta 15:793–799CrossRefGoogle Scholar
  12. Cardeal ZL, Marriott PJ (2009) Comprehensive two-dimensional gas chromatography–mass spectrometry analysis and comparison of volatile organic compounds in Brazilian cachaça and selected spirits. Food Chem 112:747–755CrossRefGoogle Scholar
  13. Cernivec S (2013) Trends in ready-to-drink tea. http://www.dairyfoods.com/articles/89259-trends-in-ready-to-drink-tea. Accessed 11 August 2016
  14. Charlebois D (2007) Elderberry as a medicinal plant. In: Janick J, Whipkey A (eds) Issues in new crops and new uses. ASHS Press, Alexandria, pp. 284–292Google Scholar
  15. Christoph N, Bauer-Christoph C (2006) Flavour of spirit drinks: raw materials, fermentation, distillation, and ageing. In: Berger RG (ed) Flavours and fragrances chemistry, bioprocessing and sustainability. Springer, Berlin, pp. 219–239Google Scholar
  16. Cordero C, Bicchi C, Rubiolo P (2008) Group-type and fingerprint analysis of roasted food matrices (coffee and hazelnut samples) by comprehensive two-dimensional gas chromatography. J Agric Food Chem 56:7655–7666CrossRefGoogle Scholar
  17. Cordero C, Kiefl J, Schieberle P, Reichenbach SE (2015) Bicchi C (2015) comprehensive two-dimensional gas chromatography and food sensory properties: potential and challenges. Anal Bioanal Chem 407:169–191CrossRefGoogle Scholar
  18. Dobrowolska-Iwanek J (2015) Simple method for determination of short-chain organic acid in mead. Food AnalMethod 8:2356–2359Google Scholar
  19. Dymerski T, Chmiel T, Mostafa A, Śliwińska M, Wiśniewska P, Wardencki W, Namieśnik J, Górecki T (2013) Botanical and geographical origin characterization of polish honeys by headspace SPME-GC × GC-TOFMS. Curr Org Chem 17:853–870CrossRefGoogle Scholar
  20. Egea T, Signorini MA, Bruschi P, Rivera D, Obón C, Alcaraz F, Palazón JA (2015) Spirits and liqueurs in European traditional medicine: their history and ethnobotany in Tuscany and bologna (Italy). J Ethnopharmacol 175:241–255CrossRefGoogle Scholar
  21. EU Agricultural Product Quality Policy. http://ec.europa.eu/agriculture/quality/index_en.htm. Accessed 11 August 2016
  22. Farkas P, Sadecka J, Kintlerova A, Kovac M, Silhar S (1995) Flavour impact compounds of fermented elder (Sambucus nigra L.) flowers macerate. In: Sontag G, Pfannhauser W (eds) Current status and future trends in analytical food chemistry, proceedings of the 8th European conference on food chemistry. Austrian Chemical Society, Vienna, pp. 329–332Google Scholar
  23. Hernández Gómez LF, Úbeda J, Arévalo-Villena M, Briones A (2009) Novel alcoholic beverages: production of spirits and liqueurs using maceration of melon fruits in melon distillates. J Sci Food Agr 89:1018–1022CrossRefGoogle Scholar
  24. Ieri F, Pinelli P, Romani A (2012) Simultaneous determination of anthocyanins, coumarins and phenolic acids in fruits, kernels and liqueur of Prunus mahaleb L. Food Chem 135:2157–2162CrossRefGoogle Scholar
  25. Jakopic J, Colaric M, Veberic R, Hudina M, Solar A, Stampar F (2007) How much do cultivar and preparation time influence on phenolics content in walnut liqueur? Food Chem 104:100–105CrossRefGoogle Scholar
  26. Jensen K, Christensen LP, Hansen M, Jørgensen U, Kaack K (2001) Olfactory and quantitative analysis of volatiles in elderberry (Sambucus nigra L) juice processed from seven cultivars. J Sci Food Agr 81:237–244CrossRefGoogle Scholar
  27. Jørgensen U, Hansen M, Christensen LP, Jensen K, Kaack K (2000) Olfactory and quantitative analysis of aroma compounds in elder flower (Sambucus nigra L.) drink processed from five cultivars. J Agric Food Chem 48:2376–2383CrossRefGoogle Scholar
  28. Journal of Laws No. 10/2005 item 68. The Act of the Ministry of Agriculture and Rural Development in Poland on the registration and protection of names and designations of agricultural products and foodstuffs and traditional products (17 December 2004). http://www.minrol.gov.pl/Jakosc-zywnosci/Produkty-regionalne-i-tradycyjne/Przepisy-polskie-Produkty-regionalne-i-tradycyjne. (in Polish) Accessed 11 August 2016
  29. Kaack K (2008) Aroma composition and sensory quality of fruit juices processed from cultivars of elderberry (Sambucus nigra L.). Eur Food Res Technol 227:45–56CrossRefGoogle Scholar
  30. Kaack K, Christensen LP (2008) Effect of packing materials and storage time on volatile compounds in tea processed from flowers of black elder (Sambucus nigra L.). Eur Food Res Technol 227:1259–1273CrossRefGoogle Scholar
  31. Magagna F, Valverde-Som L, Ruíz-Samblás C, Cuadros-Rodríguez L, Reichenbach SE, Bicchi C, Cordero C (2016) Combined untargeted and targeted fingerprinting with comprehensive two-dimensional chromatography for volatiles and ripening indicators in olive oil. Anal Chim Acta 936:245–258CrossRefGoogle Scholar
  32. Malika N, Mohamed F, Chakib E (2005) Microbiological and physic-chemical properties of Moroccan honey. Int J Agric Biol 7:773–776Google Scholar
  33. Mikova K, Havlikovi L, Velcek J, Viden I, Pudil F (1984) Neutral flavour components of elderberries and elderberry products. Lebensm-Wiss Technol 17:311–313Google Scholar
  34. Naviglio D, Montesano D, Gallo M (2015) Laboratory production of lemon liqueur (Limoncello) by conventional maceration and a two-syringe system to illustrate rapid solid–liquid dynamic extraction. J Chem Educ 92:911–915CrossRefGoogle Scholar
  35. Naviglio D, Formato A, Vitulano M, Cozzolino I, Ferrara L, Zanoelo EF, Gallo M (2016) Comparison between the kinetics of conventional maceration and a cyclic pressurization extraction process for the production of lemon liqueur using a numerical model. J Food Process Eng DOI. doi: 10.1111/jfpe.12350 Google Scholar
  36. Nikićević N, Veličković M, Jadranin M, Vučković I, Novaković M, Vujisić L, Stanković M, Urošević I, Tešević V (2011) The effects of the cherry variety on the chemical and sensorial characteristics of cherry brandy. J Serb Chem Soc 76:1219–1228CrossRefGoogle Scholar
  37. Ochmian I, Oszmiański J, Skupień K (2010) Chemical composition, phenolics, and firmness of small black fruits. J Appl Bot Food Qual 83:64–69Google Scholar
  38. Oliveira ÉR, Oliveira de Deus K, Caliari M (2015) Production, characterization and acceptability of different alcohol-based pineapple liqueurs. Revista Verde 10:108–114CrossRefGoogle Scholar
  39. Pereira AP, Mendes-Ferreira A, Oliveira JM, Estevinho LM, Mendes-Faia A (2014) Effect of Saccharomyces cerevisiae cells immobilisation on mead production. LWT-Food Sci and Technol 56:21–30CrossRefGoogle Scholar
  40. Pereira AP, Mendes-Ferreira A, Oliveira JM, Estevinho LM, Mendes-Faia A (2015) Mead production: effect of nitrogen supplementation on growth, fermentation profile and aroma formation by yeasts in mead fermentation. J Inst Brew 121:122–128CrossRefGoogle Scholar
  41. PN-64/A-04022. Methods of sensory analysis. Partial and total quality analysis by point methods. Guidelines for preparing of detailed standard assessment. Polish Committee for Standardization, Warsaw (in Polish)Google Scholar
  42. PN-A-79529-2:2005. Spirit drinks and bottled spirit—methods of tests. Guidelines for preparing of detailed standard assessment. Polish Committee for Standardization, Warsaw (in Polish)Google Scholar
  43. Poll L, Lewis MJ (1986) Volatile components of elderberry juice. Lebensm-Wiss Technol 19:258–262Google Scholar
  44. Pontes M, Marques JC, Câmara JS (2007) Screening of volatile composition from Portuguese multifloral honeys using headspace solid-phase microextraction-gas chromatography-quadrupole mass spectrometry. Talanta 74:91–103CrossRefGoogle Scholar
  45. Regulation [EC] No. 110/2008 of the European Parliament and of the Council on the definition, description, presentation, labelling and the protection of geographical indications of spirit drinks and repealing Council Regulation (EEC) No. 1576/89Google Scholar
  46. Rivellino SR, Hantao LW, Risticevic S, Carasek E, Pawliszyn J, Augusto F (2013) Detection of extraction artifacts in the analysis of honey volatiles using comprehensive two-dimensional gas chromatography. Food Chem 141:1828–1833CrossRefGoogle Scholar
  47. Samykanno K, Pang E, Marriott PJ (2013) Chemical characterisation of two Australian-grown strawberry varieties by using comprehensive two-dimensional gas chromatography–mass spectrometry. Food Chem 141:1997–2005CrossRefGoogle Scholar
  48. Schipilliti L, Bonaccorsi I, Cotroneo A, Dugo P, Mondello L (2013) Evaluation of gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) for the quality assessment of citrus liqueurs. J Agric Food Chem 61:1661–1670CrossRefGoogle Scholar
  49. Senica M, Stampar F, Veberic R, Mikulic-Petkovsek M (2016) Transition of phenolics and cyanogenic glycosides from apricot and cherry fruit kernels into liqueur. Food Chem 203:483–490CrossRefGoogle Scholar
  50. Sidor A, Gramza-Michałowska A (2015) Advanced research on the antioxidant and health benefit of elderberry (Sambucus nigra) in food—a review. J Funct Foods 18:941–958CrossRefGoogle Scholar
  51. Śliwińska M, Wiśniewska P, Dymerski T, Wardencki W, Namieśnik J (2015) The flavour of fruit spirits and fruit liqueurs: a review. Flavour Frag J 30:197–207CrossRefGoogle Scholar
  52. Śliwińska M, Wiśniewska P, Dymerski T, Wardencki W, Namieśnik J (2016a) Application of electronic nose based on fast GC for authenticity assessment of polish homemade liqueurs called nalewka. Food Anal Method 9:2670–2681CrossRefGoogle Scholar
  53. Śliwińska M, Garcia-Hernandez C, Kościński M, Dymerski T, Wardencki W, Namieśnik J, Śliwińska-Bartkowiak M, Jurga S, Garcia-Cabezon C, Rodriguez-Mendez ML (2016b) Discrimination of apple liqueurs (nalewka) using a voltammetric electronic tongue, UV-Vis and Raman spectroscopy. Sensors 16:1654–1658CrossRefGoogle Scholar
  54. Śliwińska M, Wiśniewska P, Dymerski T, Wardencki W, Namieśnik J (2016c) Advances in electronic noses and tongues for food authenticity testing. In: Downey G (ed) Advances in food authenticity testing. Woodhead Publishing, Cambridge, pp. 201–225Google Scholar
  55. Śliwińska M, Wiśniewska P, Dymerski T, Wardencki W, Namieśnik J (2016d) Evaluation of the suitability of electronic nose based on fast GC for distinguishing between the plum spirits of different geographical origins. Eur Food Res Technol 242:1813–1819CrossRefGoogle Scholar
  56. Stampar F, Solar A, Hudina M, Veberic R, Colaric M (2006) Traditional walnut liqueur—cocktail of phenolics. Food Chem 95:627–631CrossRefGoogle Scholar
  57. Stanimirova I, Üstün B, Cajka T, Riddelova K, Hajslova J, Buydens LMC, Walczak B (2010) Tracing the geographical origin of honeys based on volatile compounds profiles assessment using pattern recognition techniques. Food Chem 118:171–176CrossRefGoogle Scholar
  58. Takahashi K, Kabashima F, Tsuchiya F (2016) Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry reveals the correlation between chemical compounds in Japanese sake and its organoleptic properties. J Biosci Bioeng 121:274–280CrossRefGoogle Scholar
  59. Thole JM, Burns Kraft TF, Sueiro LA, Kang Y-H, Gills JJ, Cuendet M, Pezzuto JM, Seigler DS, Lila MA (2006) A comparative evaluation of the anticancer properties of European and American elderberry fruits. J Med Food 9:498–504CrossRefGoogle Scholar
  60. Traditional Polish Products. The list of regional and traditional products of the Ministry of Agriculture and Rural Development in Poland. http://www.minrol.gov.pl/Jakosc-zywnosci/Produkty-regionalne-i-tradycyjne/Lista-produktow-tradycyjnych/woj.-pomorskie/Nalewka-Onisiowka. (in Polish) Accessed 11 August 2016
  61. Van Den Dool H, Kratz PD (1963) A generalization of the retention index system including linear temperature programmed gas-liquid partition chromatography. J Chromatogr A 11:463–471CrossRefGoogle Scholar
  62. Vázquez-Araújo L, Rodríguez-Solana R, Cortés-Diéguez SM, Domínguez JM (2013) Study of the suitability of two hop cultivars for making herb liqueurs: volatile composition, sensory analysis, and consumer study. Eur Food Res Technol 237:775–786CrossRefGoogle Scholar
  63. Villière A, Arvisenet G, Lethuaut L, Prost C, Sérot T (2012) Selection of a representative extraction method for the analysis of odourant volatile composition of French cider by GC–MS–O and GC×GC–TOF-MS. Food Chem 131:1561–1568CrossRefGoogle Scholar
  64. Vítová E, Sůkalová K, Mahdalová M, Butorová L, Babák L, Matějíček A (2015) Comparison of flavour and volatile flavour compounds of mixed elderberry juices. Acta Univ Agric et Silvic Mendel Brun 63:147–152CrossRefGoogle Scholar
  65. ‘Wędrowna Barć’. Official website of the farmhouse ‘Wędrowna Barć’ http://www.pasieka-krzemienica.pl/. (in Polish) Accessed 11 August 2016
  66. Weldegergis BT, de Villiers A, McNeish C, Seethapathy S, Mostafa A, Górecki T, Crouch AM (2011) Characterisation of volatile components of Pinotage wines using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GCxGC–TOFMS). Food Chem 129:188–199CrossRefGoogle Scholar
  67. Welke JE, Alcaraz Zini C (2011) Comprehensive two-dimensional gas chromatography for analysis of volatile compounds in foods and beverages. J Braz Chem Soc 22:609–622CrossRefGoogle Scholar
  68. Welke JE, Manfroi V, Zanus M, Lazarotto M, Alcaraz Zini C (2012) Characterization of the volatile profile of Brazilian merlot wines through comprehensive two dimensional gas chromatography time-of-flight mass spectrometric detection. J Chromatogr A 1226:124–139CrossRefGoogle Scholar
  69. Welke JE, Zanus M, Lazzarotto M, Alcaraz Zini C (2014a) Quantitative analysis of headspace volatile compounds using comprehensive two-dimensional gas chromatography and their contribution to the aroma of chardonnay wine. Food Res Int 59:85–99CrossRefGoogle Scholar
  70. Welke JE, Zanus M, Lazzarotto M, Pulgati FH, Alcaraz Zini C (2014b) Main differences between volatiles of sparkling and base wines accessed through comprehensive two dimensional gas chromatography with time-of-flight mass spectrometric detection and chemometric tools. Food Chem 164:427–437CrossRefGoogle Scholar
  71. Winterová R, Mikulíková R, Mazáč J, Havelec P (2008) Assessment of the authenticity of fruit spirits by gas chromatography and stable isotope ratio analyses. Czech J Food Sci 26:368–375Google Scholar
  72. Yao F, Yi B, Shen C, Tao F, Liu Y, Lin Z, Xu P (2015) Chemical analysis of the Chinese liquor Luzhoulaojiao by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry. Sci Rep 5:9553–9559CrossRefGoogle Scholar
  73. Zhu S, Lu X, Ji K, Guo K, Li Y, Wu C, Xu G (2007) Characterization of flavor compounds in Chinese liquor Moutai by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry. Anal Chim Acta 597:340–348CrossRefGoogle Scholar

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© The Author(s) 2016

Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.

Authors and Affiliations

  • Magdalena Śliwińska
    • 1
  • Paulina Wiśniewska
    • 1
  • Tomasz Dymerski
    • 1
  • Waldemar Wardencki
    • 1
  • Jacek Namieśnik
    • 1
  1. 1.Department of Analytical Chemistry, Faculty of ChemistryGdansk University of TechnologyGdańskPoland

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