Quantitative Determination of Arsenic Species from Fruit Juices Using Acidic Extraction with HPLC-ICPMS

  • Kevin M. KubachkaEmail author
  • Sean D. Conklin
  • Cynthia C. Smith
  • Consuelo Castro


Throughout the US Food and Drug Administration’s routine monitoring of various juice samples for elemental contaminants, a limited number of samples exhibited unexpected behavior related to the arsenic content. Juice samples were subjected to total arsenic determination and those containing arsenic > 10 μg kg−1 were subjected to arsenic speciation analysis using FDA Elemental Analysis Manual (EAM) 4.10 method (AOAC First Action Method 2016.04) to determine the concentration of iAs and other common organic arsenicals. For a subset of samples, the sum of the arsenic species was significantly less than the total arsenic value (i.e., mass balance < 65%), which is uncommon for a liquid-based matrix. Juice types that have exhibited this behavior include pomegranate, prune, and cherry juices. Causes for this issue were explored which ultimately led to an alternate sample preparation technique, extraction with 0.28 M HNO3 along with heat, which resulted in drastically improved mass balances approaching 100%. The method proved robust, with both accurate and precise measurements for multiple juice samples analyzed by a total of four laboratories. Two laboratories performed a level 3 multilaboratory validation. This work discusses various issues that were encountered, attempts to determine the source of the problem, the eventual solution in the form of a modified extraction procedure, and the multilaboratory validation results.


Juice Arsenic Speciation Mass balance HPLC-ICPMS 



The authors would like to thank the analysts from the FDA laboratories that analyzed the samples as part of the multilaboratory study, Miranda McDonald from the Kansas City Lab Laboratory, in Lenexa, KS, as well as Christina Qiu from the San Francisco Laboratory, in Alameda, CA. Additionally, the authors would like to thank Diana Mould from the Southeast Food and Feed Laboratory for data regarding pomegranate juice samples analyzed utilizing the extraction method.

Compliance with Ethical Standards


The views expressed in this article are those of the authors and do not necessarily reflect the views or policies of the US Food and Drug Administration. Mention of trade names or commercial products does not constitute endorsement or recommendation for use.

Conflict of Interest

Kevin M. Kubachka declares that he has no conflict of interest. Sean D. Conklin declares that he has no conflict of interest. Cynthia Smith declares that she has no conflict of interest. Consuelo Castro declares that she 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.

Informed Consent

Not applicable


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Copyright information

© This is a U.S. Government work and not under copyright protection in the US; foreign copyright protection may apply 2019

Authors and Affiliations

  1. 1.Forensic Chemistry Center, US FDACincinnatiUSA
  2. 2.Center for Food Safety and Applied Nutrition, US FDACollege ParkUSA
  3. 3.Kansas City Laboratory, US FDALenexaUSA
  4. 4.San Francisco Laboratory, US FDAAlamedaUSA

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