Abstract
Composition and purity are critical to safety and performance of food emulsifiers. Wet chemical methods such as titrations, color, and melting points have been used since the early twentieth century. These methods are inexpensive and well accepted. On the other hand, they generate large volumes of waste solvents and require skilled analysts. Modern instrumental methods use small samples, can be automated, and are less subjective. Their disadvantages are equipment expense and maintenance costs.
Separation technologies such as gas-liquid chromatography and high performance liquid chromatography are useful for determining composition. Nuclear magnetic resonance, ultraviolet and infrared spectroscopy, and mass spectrometry provide detailed structural information. Combinations of technologies can completely characterize a complex emulsifier mixture.
Some analytical specifications are mandated by government agencies and trade associations. In most cases they are negotiated by the supplier and food manufacturer. Setting reliable specifications can ensure good performance, safety, and fewer product recalls.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Blanco M et al (2004) Analytical control of an esterification batch reaction between glycerine and fatty acids by near-infrared spectroscopy. Anal Chem Acta 521(13):143–148
Bosco M et al (1997) Organic solvent systems for 31P nuclear magnetic resonance analysis of lecithin phospholipids: applications to two-dimensional gradient-enhanced 1H-detected heteronuclear multiple quantum coherence experiments. Anal Biochem 245(1):38–47
Bruemmer J (1971) Brot Gebaeck 25(11):217–220
Bruschweiler H, Dieffenbacher A (1991) Determination of mono- and diglycerides by capillary gas chromatography: results of a collaborative study and the standardized method. Pure Appl Chem 63(8):1153–1162
Byrdwell W (2005a) Modern methods for lipid analysis by liquid chromatography/mass spectrometry and related techniques. AOCS Press, Champaign
Byrdwell W (2005b) Atmospheric ionization techniques in modern lipid analysis. In: Byrdwell W (ed) Modern methods of lipid analysis. AOCS Press, Champaign, pp 1–18
Byrdwell W (2005c) Dual parallel liquid chromatography/mass spectrometry for lipid analysis. In: Byrdwell W (ed) Modern methods for lipid analysis. AOCS Press, Champaign, pp 510–576
Cai S, Syage I (2006) J Chromatogr AII 10:15–26
Christie W (1992) Detectors for high performance liquid chromatography of lipids with special reference to evaporative light scattering detection. In: Christie W (ed) Advances in lipid methodology. The Oily Press, Ayr, Scotland
Christie W (1996) Separation of phospholipid classes by high performance chromatography. Advances in lipid methodology, vol 3. The Oily Press, Bridgwater, pp 77–108
Christie W, Ha X (2010) Lipid analysis: isolation, separation, identification, and lipidomic analysis4th edn. The Oily Press, Bridgwater
Cruz R (2014) Methods in food analysis. CRC Press, New York
Dang H (2006) Composition analysis of two batches of polysorbate 60 using MS and NMR techniques. J Pharm Biomed Anal 40(5):1155–1165
Daniels D (1982) J Assoc Offic Anal Chem 65(1):162–165
Daniels D et al (1985) J Agric Food Chem 33(3):368–372
DeMeulenaer B et al (2000) Combined liquid and gas chromatographic characterisation of polyglycerol fatty acid esters. J Chromatogr 896(1–2):239–251
Dieffenbacher A (1989) Rev Fr Corps Gras 36(2):64
Diepenmaat-Walters M et al (1997) J Am Soc Brew Chem 55(4):147–152
Duden R, Fricker A (1977) Dünnschichtchromatographische Bestimmung von Mono- und Digalactosyldiglyceriden sowie Lecithinen in Spinat. Fettee Seifen Anstrichm 79(12):489–491
Ekoos K (2012) Lippidomics: technologies and applications. Wiley-VCH
Everts F, Davis J (2000) 1H and 13C NMR of multilamellar dispersions of polyunsaturated (22:6) phospholipids. Biophys J 79(2):885–887
Fanali S et al (2013) Liquid chromatography: applications. Elsevier, Amsterdam
Federal Register (2013) Code of Federal Regulations, title 21, food and drug, Sections 172, 182, 184
Filip V, Kleunova M (1993) Bestimmung von Mono-, Di- und Triglyceriden mit HPLC. Z Lebensmit Unters Forsch 196(6):532–535
Firestone D (2013a) Official methods and recommended practices of the AOCS6th edn., third printing. AOCS Publications, Champaign, IL
Firestone D (2013b) Method Cd 11-57: α-monoglyceride
Firestone D (2013c) Method Cd 3d-63: acid value of fats and oils; Method Ja 6-55: acid value of lecithin
Firestone D (2013d) Methods Cd 1-25: iodine value of fats and oils; Ja 14-91: iodine value of lecithin
Firestone D (2013e) Method Cd 8b-90: peroxide value using isooctane; Ja 8-87: peroxide value of lecithin
Firestone D (2013f) Method Cd 3c-91: saponification value of fats and oils, modified using methanol
Firestone D (2013g) Method Cd 14-40: hydroxyl value of fats and oils (acetyl value); cd 13-60: hydroxyl value of fatty oils and alcohols
Firestone D (2013h) Method Cd 5-40: Reichert-Meisel value
Firestone D 2013i) Method Ca 2e-84: moisture by Karl Fischer method in fats & oils
Firestone D (2013j) Method Tb 2-64: moisture by Karl fisher method in industrial oil derivatives. Method Ja 2b-87: moisture by Karl Fischer method in lecithin
Firestone D (2013k) Method Cc 17-95: soap in oil
Firestone D (2013l) Method Ca 12a-02: colorimetric determination of phosphorus in fats and oils
Firestone D (2013m) Methods Cc 13b-45, color: Lovibond (Wesson), and cc 13e-92, color: lovibond (ISO standard)
Firestone D (2013n) Methods Td 1a-64, color: gardner (industrial oils) and Ja 9-87, color: gardner (lecithin)
Firestone D (2013o) Method Cc 13j-97, color (automated method)
Firestone D (2013p) Method Cc 13a-43, color (FAC)
Firestone D (2013q) Method Cc 13c-50, color (spectrophotometric method for oils)
Firestone D (2013r) Method Cc 7-25 refractive index (fats and oils)
Firestone D (2013s) Method Cc1-25, melting point: capillary tube method
Firestone D (2013t) Method Cc 3-25, slip melting point (AOCS Standard); method Cc 3b-92: slip melting point (ISO method)
Firestone D (2013u) Method Cc 18-80, mettler dropping point
Firestone D (2013v) Methods Ja 11-7, viscosity: lecithin (bubble time method); and Da 26-42, viscosity: transparent liquids (bubble time method)
Firestone D (2013w) Method Ja 10-87, viscosity: lecithin (Brookfield)
Firestone D (2013x) Method Cc 10a-25 specific gravity of liquid oils and fats
Firestone D (2013y) Method Cc 10b-25: specific gravity of solid fats and waxes
Firestone D (2013z) Method Ce 1-62: fatty acid composition by GLC of methyl esters; method Cd 28-10: glyceryl fatty acid esters in edible oil
Firestone D (2013aa) Method Cd 11b-91: mono- and diglycerides by capillary GLC
Firestone D (2013ab) Method Cd 11d-96: Mono- and diglycerides by HPLC – ELSD
Firestone D (2013ac) Method Ja 7b-91: phospholipids in lecithin concentrates by HPLC; Method Ja 7c-07: phospholipids in lecithin concentrates by HPLC-ELSD
Firestone D (2013ad) Method Ca 14b-96: free glycerin by HPLC-ELSD
Firestone D (2013ae) Method Cd 25a-00: heat exchange fluid by HPLC
Firestone D (2013af) Method Ca 12a-02: phosphorus in oils (ISO Method)
Firestone D (2013ag) Method Cd 1e-01: iodine value by NIR
Firestone D (2013ah) Method Ca 18-91: lead in oils – graphite furnace
Firestone D (2013ai) Methods 15–75: iron, copper, and chromium by AAS; Ca 18-79: iron, copper, and chromium in oils by AAS - graphite furnace
Firestone D (2013aj) Method Ca 17-01: trace metals by ICP-ECS
Firestone D (2013ak) Method Cd 16b-93: solid fat content (SFC) by low-resolution nuclear magnetic resonance (direct method); and Cd 16-81: solid fat content (SFC) by low-resolution nuclear resonance (indirect method)
Franzke C (1977) Z Lebensm Unters Forsch 163(3):206–207
Franzke C, Kroll J (1980) Zur enzymatischen milchsäurebestimmung in emulgatoren. Nahrung 24(1):89–90
Frison-Norrie S (2001) Investigating the molecular heterogeneity of polysorbate emulsifiers by MALDI-TOF MS. J Agric Food Chem 49(7):3335–3340
Gaonkar A, McPherson A (2005) Ingredient interactions: effects on food quality. CRC Press, Boca Raton
Garti N (1981) J Liq Chromatogr 94(7):1173–1194
Garti N, Acerin A (1983) J Am Oil Chem Soc 690(6):1151–1154
Gillet B et al (1998) Analysis 26(3):M26–M33
Glonek T, Merchant R (1996) 31P nuclear magnetic resonance profiling of phospholipids. In: Christie W (ed) Advances in lipid methodology, vol 3. The Oily Press, Ayr, Scotland, pp 37–75
Grdadolnik J, Hadm D (1993) Conformational effects of metal salt binding to the polar head of phosphatidylcholines investigated by FTIR spectroscopy. Chem Phys Lipids 65(2):121–132
Gross H (2011) Mass spectrometry: a textbook2nd edn. Springer, Heidelberg
Gunstone F (1993) High resolution 13C NMR spectroscopy of lipids. In: Christie W (ed) Advances in lipid methodology, vol 2. The Oily Press, Ayr, Scotland, pp 1–68
Hammond E (1993) Chromatography for the analysis of lipids. CRC Press, Boca Raton
Han X, Gross R (2005) Toward total cellular lipidome analysis by ESI mass spectrometry from a crude lipid extract. In: Byrdwell W (ed) Modern methods of lipid analysis. AOCS Press, Champaign, pp 488–509
Hartman l et al (1980) Method for the determination of phosphorus in lipids and lipid-containing materials. Analyst 105(1247):173–176
Hasenhuettl G et al (1990) J Am Oil Chem Soc 67(11):797–799
Hore P (2015) Nuclear magnetic resonance. Oxford University Press, Oxford
Hsieh J et al (1981) General method for the analysis of phosphatidylcholines by high-performance liquid chromatography. J Chromatogr 208(2):398–403
Hummel D (2000a) Handbook of surfactant analysis. John Wiley & Sons, New York, p 232
Hummel P (2000b) p 233
Hurst W, Martin R (1984) The analysis of phospholipids in soy lecithin by HPLC. J Am Oil Chem Soc 61(9):1462–1463
Huyghebaert G, Baert L (1992) Chromatographia 34(11–12):557–562
Indrastri D (2010) J Am Oil Chem Soc 87:1257–1262
Ingber N (1986) Unpublished Research
Istratov V et al (2003) Linear-dendritic nonionic poly(propylene oxide)–polyglycerol surfactants. Tetrahedron 59(22):4017–4024
Iwasaki Y et al (2013) J Am Oil Chem Soc 90(7):951–957
Jakubska E et al (1977) Axta Aliment Pol 3(1):79–84
Jodlbauer D (1981) Veroeff Arbeitsgen Getreideeforsch 53(8):42–49
Kaitaranta J, Bessman S (1981) Anal Chem 55(8):1232–1235
Karrer R, Herberg H (1992) Analysis of sucrose fatty acid esters by high temperature gas chromatography. J High Res Chromatogr 15(9):585–589
Kato H et al (1989) J Assoc Offic Anal Chem 72(1):27–29
Kostelnik R, Costellano S (1973) J Magn Reson 9(2):291–295
Kumar T et al (1984) J Chromatogr A 398:360–365
Larsen A, Hyattumff E (2005) Analysis of phospholipids by liquid chromatography coupled with online electrospray ionization mass spectrometry and tandem mass spectrometry. In: Byrdwell W (ed) Modern methods of lipid analysis. AOCS Press, Champaign, IL, pp 19–60
Latimer G (2012) Official methods of analysis of AOAC19th edn. AOAC International, Gaithersburg, MD
Lee T (1988) J Assoc Off Anal Chem 71(4):785–788
Lee T et al (1993) J Am Oil Chem Soc 70(4):343–347
Lew H (1975) Veroff. Landwirtsch Chem Bundesversuchsanst Linz 97(10):10
Li Y-K et al (2002) Sepu 20(5):476–478
Li H et al (2009) Fourier transform near infrared spectroscopy as a quality control tool for the analysis of lecithin and by-products during soybean oil processing. J Am Oil Chem Soc 86(9):835–841
Lindblom G (1996) Nuclear magnetic spectroscopy, lipid phase behavior, and lipid diffusion. In: Christie W (ed) Advances in lipid methodology, vol 3. The Oily Press, Ayr, Scotland, pp 132–199
Lundquist G, Meloan C (1971) Determination of polysorbates in food products by reaction gas chromatography. Anal Chem 43(8):1122–1123
Luquain C et al (2001) High-performance liquid chromatography determination of Bis(monoacylglycerol) phosphate and other lysophospholipids. Anal Biochem 296(1):41–48
Macka M et al (1994) Analysis of silanised polyglycerols by supercritical fluid chromatography. J Chromatogr 675(1–2):267–270
Mazur A et al (1991) Regio- and stereoselective enzymatic esterification of glycerol and its derivatives. Chem Phys Lipids 60(2):189–199
Melton S (1992) Analysis of soybean lecithins and beef phospholipids by HPLC with an evaporative light scattering detector. J Am Oil Chem Soc 69(8):784–788
Moelering H, Bergmeyer HU (1974) Methoden Enzym Anal 3. In: Bergenmeyer H (ed) Neubearbeitete Erweite Te Auft, vol 2. Academic Press, New York, pp 1860–1864
Mueller H (1977) Die Gehalte an Lecithin und anderen Cholin-Verbindungen in Nahrungspflanzen. Fette Seifen Annstrichm 79(6):259–261
Murakami C et al (1989) Determination of sucrose esters of fatty acids by high performance liquid chromatography. Shokuhin Eiseigaku Zasshi 30(4):306–315
Murgia S et al (2003) Quantitative characterization of phospholipids in milk fat via 31P NMR using a monophasic solvent mixture. Lipids 38(5):585–591
Murphy R, Gaskell S (2014) Tandem mass spectrometry of lipids: molecular analysis of complex lipids. Royal Society of Chemistry, London
Murphy J, Grislett L (1969) J Am Oil Chem Soc 76(7):384
Nakanishi H, Tsuda T (1983) Gas-liquid chromatographic determination of monoglycerides in foods. Shokuhin Eisergaku Zasshi 24(5):474–479
Nunez A et al (2005) Liquid chromatography/mass spectrometry analysis of biosurfactant glycolipids. In: Byrdwell W (ed) Modern methods for lipid analysis. AOCS Press, Champaign, IL, pp 447–471
Olsson U et al (1990) J Planar Chromatogr - Mod TLC 3:55–60
Orfanakis A et al (2013) Characterization of polyglycerol polyricinoleate formulations using NMR spectroscopy, mass spectrometry and dynamic light scattering. J Am Oil Chem Soc 90:39–51
Pohle W et al (1997) J Mol Struct 408–409:273–277
Poole C (2014) Instrumental thin-layer chromatography. Elsevier, Amsterdam
Press K et al (1981) Comparison of high-performance liquid chromatography and proton nuclear magnetic resonance in determining the phosphatidylcholine content in soy lecithin. J Agric Food Chem 29(5):1096–1098
Ranger RR, Wenz K (1989) J Planar Chromatogr – Mod TLC 2(1):24–27
Regula E (1975) Dünnschichtchromatographischer nachweis von calcium- und natrium-stearoyllactylat neben anderen emulgatoren in lebensmitteln. J Chromatogr 115(2):639–644
Rhee J, Shin M (1982) Analysis of phosphatidylcholine in soy lecithins by HPLC. J Am Oil Chem Soc 59(2):98–99
Sacchi P et al (1990) Revista Italiano delle Sostanze Grasse 67(5):245–252
Saito K et al (1987) Determination of polysorbates in powdered soup packed in commercially imported instant noodles. Shokuhin Eisaigaku Zasshi 28(5):372–377
Schmidt M (1976) Offenders. Getreide Mehl Brot 30(3):62–64
Schutze T (1977) Analytische Charakterisierung von Polyglycerinester-Emulgatoren. Nahrung 21(5):405–415
Schuyl P, VanPlaterink C (1994) Analysis of sucrose polyesters with electrospray mass spectrometry. 42nd ASMS Conference on Mass Spectrometry, Chicago, IL
Senelt S et al (1986) Turrk Hij Deney Biyol Derg 43(1):23–45
Sheeley D et al (1986) Spectroscopy 1(2):38–39
Shmidt A (1979) Lebensmittelindustrie 26(4):172–173
Sotirhos N et al (1986) Dev Food Sci 12:601–608
Tajano S, Kondoh Y (1987) Monoglyceride analysis with reversed phase HPLC. J Am Oil Chem Soc 64(7):1001–1003
Takagi T, Ando Y (1994) Separation of monoacylglycerols by high-performance liquid chromatography on nitrile-bonded phase. J Am Oil Chem Soc 71(4):459–460
Tanaka M et al (1979) Yukagaku 28(2):96–99
Tasumi M (2014) Introduction to experimental infrared spectroscopy: fundamentals and practical methods. Wiley, New York
Tonogau Y et al (1987) Detection and determination of polysorbate in powdered soup of instant noodles by colorimetry. Shokuhin Eisaigaku Zasshi 28(6):427–435
Trautler H, Nikiforov A (1984) Anal Chem Symp Ser 21:299–304
Tsuda T et al (1984) J AOAC Int 84(2):498–506
Tumanaka K, Fujita N (1990) Yukagaku 19(6):393–397
Uematsu Y et al (2001) Determination of sucrose esters of fatty acids in food additive premixes by gas chromatography and confirmation of identity by gas chromatography/mass spectrometry. J AOAC Int 84(2):498–506
Watanabe M et al (1986) Yakagaku 35(12):1018–1024
Yamanaka S, Kudo K (1991) CA 115:123048. Japan 03107765
Yusupoca I, et al. (1976) Khim. Prom-St. 598-600, CA 88: 35919
Acknowledgements
This chapter was written with fond memories of Nate Ingber, who had an incredible talent for applying modern instrumental techniques to difficult analytical challenges. The author is indebted to Julia Hasenhuettl and Shirley Moore for their dedicated efforts in literature searches and manuscript preparation.
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2019 Springer Nature Switzerland AG
About this chapter
Cite this chapter
Hasenhuettl, G.L. (2019). Analysis of Food Emulsifiers. In: Hasenhuettl, G., Hartel, R. (eds) Food Emulsifiers and Their Applications. Springer, Cham. https://doi.org/10.1007/978-3-030-29187-7_3
Download citation
DOI: https://doi.org/10.1007/978-3-030-29187-7_3
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-030-29185-3
Online ISBN: 978-3-030-29187-7
eBook Packages: Biomedical and Life SciencesBiomedical and Life Sciences (R0)