<?xml version="1.0" encoding="UTF-8"?>
<!DOCTYPE article PUBLIC "-//NLM//DTD JATS (Z39.96) Journal Publishing DTD v1.3 20210610//EN" "JATS-journalpublishing1-3.dtd">
<article article-type="research-article" dtd-version="1.3" xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance" xml:lang="ru"><front><journal-meta><journal-id journal-id-type="publisher-id">rfhealth</journal-id><journal-title-group><journal-title xml:lang="ru">Здравоохранение Российской Федерации</journal-title><trans-title-group xml:lang="en"><trans-title>Health care of the Russian Federation</trans-title></trans-title-group></journal-title-group><issn pub-type="ppub">0044-197X</issn><issn pub-type="epub">2412-0723</issn><publisher><publisher-name>Federal Scientific Center of Hygiene named after F.F. Erisman</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.47470/0044-197X-2021-65-4-388-393</article-id><article-id custom-type="elpub" pub-id-type="custom">rfhealth-502</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Article</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="ru"><subject>ТОКСИКОЛОГИЯ (ПРОФИЛАКТИЧЕСКАЯ, КЛИНИЧЕСКАЯ, ЭКОЛОГИЧЕСКАЯ)</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="en"><subject>TOXICOLOGY (PREVENTIVE, CLINICAL, ECOLOGICAL)</subject></subj-group></article-categories><title-group><article-title>Безопасность пищевой продукции: современные приёмы многокомпонентного определения пестицидов</article-title><trans-title-group xml:lang="en"><trans-title>Food safety: modern methods of multicomponent determination of pesticides</trans-title></trans-title-group></title-group><contrib-group><contrib contrib-type="author" corresp="yes"><contrib-id contrib-id-type="orcid">https://orcid.org/0000-0002-9959-6507</contrib-id><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Ракитский</surname><given-names>В. Н.</given-names></name><name name-style="western" xml:lang="en"><surname>Rakitskii</surname><given-names>Valerii N.</given-names></name></name-alternatives><xref ref-type="aff" rid="aff-1"/></contrib><contrib contrib-type="author" corresp="yes"><contrib-id contrib-id-type="orcid">https://orcid.org/0000-0001-8278-6382</contrib-id><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Федорова</surname><given-names>Наталия Евгеньевна</given-names></name><name name-style="western" xml:lang="en"><surname>Fedorova</surname><given-names>Natalia E.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Доктор биол. наук, гл. науч. сотр., зав. отделом аналитических методов контроля ФБУН «Федеральный научный центр гигиены им. Ф.Ф. Эрисмана» Роспотребнадзора, 141014, Мытищи, Московская область.</p><p>e-mail: fedorovane@fferisman.ru</p></bio><bio xml:lang="en"><p>Dr. Sci. Biol., Federal Scientific Center of Hygiene named after F.F. Erisman, Federal Service for Surveillance on Consumer Rights Protection and Human Wellbeing, Mytishchi, Moscow Region, 1410014, Russian Federation.</p><p>e-mail: fedorovane@fferisman.ru </p></bio><email xlink:type="simple">fedorovane@fferisman.ru</email><xref ref-type="aff" rid="aff-1"/></contrib></contrib-group><aff-alternatives id="aff-1"><aff xml:lang="ru">ФБУН «Федеральный научный центр гигиены имени Ф.Ф. Эрисмана» Федеральной службы по надзору в сфере защиты прав потребителей и благополучия человека<country>Россия</country></aff><aff xml:lang="en">Federal Scientific Center of Hygiene named after F.F. Erisman of the Federal Service for Surveillance on Consumer Rights Protection and Human Wellbeing<country>Russian Federation</country></aff></aff-alternatives><pub-date pub-type="collection"><year>2021</year></pub-date><pub-date pub-type="epub"><day>03</day><month>09</month><year>2021</year></pub-date><volume>65</volume><issue>4</issue><fpage>388</fpage><lpage>393</lpage><permissions><copyright-statement>Copyright &amp;#x00A9; Ракитский В.Н., Федорова Н.Е., 2021</copyright-statement><copyright-year>2021</copyright-year><copyright-holder xml:lang="ru">Ракитский В.Н., Федорова Н.Е.</copyright-holder><copyright-holder xml:lang="en">Rakitskii V.N., Fedorova N.E.</copyright-holder><license license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>This work is licensed under a Creative Commons Attribution 4.0 License.</license-p></license></permissions><self-uri xlink:href="https://www.rfhealth.ru/jour/article/view/502">https://www.rfhealth.ru/jour/article/view/502</self-uri><abstract><sec><title>Введение</title><p>Введение. Аналитический контроль химической контаминации имеет существенное значение в вопросах обеспечения безопасности пищевой продукции, произведённой с применением пестицидов. Развитие и апробация новых методических приёмов мультикомпонентного измерения уровней остаточных количеств биологически активных ингредиентов постоянно находятся в поле зрения аналитиков.</p><p>Цель исследования – выполнить оценку пригодности методических подходов QuEChERS для определения широкого спектра пестицидов различной структуры и физико-химических свойств (до 50 наименований действующих веществ) в пищевой продукции и продовольственном сырье различного состава и происхождения (фрукты, овощи, зерно хлебных злаков, рис, чай, кофе, молоко, яйца и продукты их переработки, мясо, субпродукты).</p></sec><sec><title>Материал и методы</title><p>Материал и методы. Измерения выполнены методами тандемной жидкостной хромато-масс-спектрометрии, а также газовой хроматографии с масс-селективным детектором, ориентированными на скрининг и количественное определение следовых количеств пестицидов. Процедура пробоподготовки образцов к анализу проведена по методике QuEChERS. </p></sec><sec><title>Результаты</title><p>Результаты. Созданы мультиметоды определения остаточных количеств пестицидов в зерне хлебных злаков (40 веществ), плодах овощей и фруктов (27 соединений), плодах цитрусовых культур (50 ингредиентов), 2,4-Д-кислоты в молоке, яйцах и субпродуктах, фипронила и его токсичного метаболита – сульфона в яйцах, продуктах их переработки (меланж, сухой яичный белок), мышечной ткани и субпродуктах. Разработки дополнили перечень аттестованных методов измерений, включенных в единый информационный фонд методик измерений Российской Федерации. </p></sec><sec><title>Выводы</title><p>Выводы. Унификация аналитических приемов подготовки к анализу проб пищевой продукции различного состава и происхождения, приборное оснащение аналитических лабораторий системами жидкостной и газовой хромато-масс-спектрометрии расширяют возможности внедрения групповых методов, обеспечивают готовность испытательных центров к выполнению мультицелевых испытаний по выявлению и измерению уровней пестицидов.</p></sec></abstract><trans-abstract xml:lang="en"><sec><title>Introduction</title><p>Introduction. Analytical control of chemical contamination is essential in ensuring the safety of food products manufactured using pesticides. The development and testing of new methodological techniques for multicomponent measurement of the levels of residual amounts of biologically active ingredients are constantly in the field of view of analysts.</p></sec><sec><title>Research objectives</title><p>Research objectives. To assess the suitability of the QuEChERS methodological approaches for the determination of a wide range of pesticides of various structures and physicochemical properties (up to 50 names of active substances) in food products and food raw materials of various compositions and origins (fruits, vegetables, cereals, rice, tea, coffee, milk, eggs and their derivatives, meat, offal).</p></sec><sec><title>Material and methods</title><p>Material and methods. The measurements were carried out by tandem liquid chromatography-mass spectrometry and gas chromatography with a mass-selective detector, focused on screening and quantifying trace amounts of pesticides. The sample preparation procedure for analysis was carried out according to the QuEChERS method. </p></sec><sec><title>Results</title><p>Results. Multimethods have been created for the determination of residual amounts of pesticides in cereal grains (40 substances), fruits of vegetables and fruits (27 compounds), fruits of citrus crops (50 ingredients), 2,4-D acid in milk, eggs and by-products, fipronil and its toxic metabolite – sulfone in eggs, products of their processing (melange, dry egg white), muscle tissue and offal. The developments have supplemented the list of certified measurement methods included in the unified information fund of measurement methods of the Russian Federation.</p></sec><sec><title>Conclusions</title><p>Conclusions. The unification of analytical methods for preparing samples of food products of various composition and origin for analysis, instrumentation of analytical laboratories with liquid and gas chromatography-mass spectrometry systems expand the possibilities of introducing group methods, ensure the readiness of testing centres to perform multi-purpose tests to identify and measure pesticide levels.</p></sec></trans-abstract><kwd-group xml:lang="ru"><kwd>пищевая продукция</kwd><kwd>остаточные количества пестицидов</kwd><kwd>мультикомпонентное определение</kwd></kwd-group><kwd-group xml:lang="en"><kwd>food products</kwd><kwd>pesticide residues</kwd><kwd>multicomponent determination</kwd></kwd-group></article-meta></front><back><ref-list><title>References</title><ref id="cit1"><label>1</label><citation-alternatives><mixed-citation xml:lang="ru">CODEX Online Glossary of Terms. Available at: https://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/pestres/glossary/en/</mixed-citation><mixed-citation xml:lang="en">CODEX Online Glossary of Terms. Available at: https://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/pestres/glossary/en/</mixed-citation></citation-alternatives></ref><ref id="cit2"><label>2</label><citation-alternatives><mixed-citation xml:lang="ru">Food Safety Authority (EFSA). The 2019 European Union report on pesticide residues in Food. EFSA Journal. 2021; 19(4): 6491. https://doi.org/10.2903/j.efsa.2021.6491</mixed-citation><mixed-citation xml:lang="en">Food Safety Authority (EFSA). The 2019 European Union report on pesticide residues in Food. EFSA Journal. 2021; 19(4): 6491. https://doi.org/10.2903/j.efsa.2021.6491</mixed-citation></citation-alternatives></ref><ref id="cit3"><label>3</label><citation-alternatives><mixed-citation xml:lang="ru">Клисенко М.А., ред. Методы определения микроколичеств пестицидов в продуктах питания, кормах и внешней среде. М.: Агропромиздат; 1992.</mixed-citation><mixed-citation xml:lang="en">Klisenko M.A., ed. Methods for the Determination of Trace Amounts of Pesticides in Food, Feed and the Environment [Metody opredeleniya mikrokolichestv pestitsidov v produktakh pitaniya, kormakh i vneshney srede]. Moscow: Agropromizdat; 1992. (in Russian)</mixed-citation></citation-alternatives></ref><ref id="cit4"><label>4</label><citation-alternatives><mixed-citation xml:lang="ru">Исаев Л.К., ред. Контроль химических и биологических параметров окружающей среды. СПб.: Союз; 1998.</mixed-citation><mixed-citation xml:lang="en">Isaev L.K., ed. Control of Chemical and Biological Parameters of the Environment [Kontrol’ khimicheskikh i biologicheskikh parametrov okruzhayushchey sredy]. St. Petersburg: Soyuz; 1998. (in Russian)</mixed-citation></citation-alternatives></ref><ref id="cit5"><label>5</label><citation-alternatives><mixed-citation xml:lang="ru">Hogenboom A.C., Niessen W.M.A., Brinkman U.A.T. The role of column LC-MS in environmental trace-level analysis. J. Sep. Sci. 2001; 24: 331.</mixed-citation><mixed-citation xml:lang="en">Hogenboom A.C., Niessen W.M.A., Brinkman U.A.T. The role of column LC-MS in environmental trace-level analysis. J. Sep. Sci. 2001; 24: 331.</mixed-citation></citation-alternatives></ref><ref id="cit6"><label>6</label><citation-alternatives><mixed-citation xml:lang="ru">Budde W.L. Analytical mass spectrometry of herbicides. Mass Spectrom. Rev. 2004; 23(1): 1–24.</mixed-citation><mixed-citation xml:lang="en">Budde W.L. Analytical mass spectrometry of herbicides. Mass Spectrom. Rev. 2004; 23(1): 1–24.</mixed-citation></citation-alternatives></ref><ref id="cit7"><label>7</label><citation-alternatives><mixed-citation xml:lang="ru">Picό Y., Blasco C., Font G. Environmental and food applications of LC-MS-MS in pesticide-residue analysis: an overview. Mass Spectrom. Rev. 2004; 23(1): 45–85. https://doi.org/10.1002/mas.10071</mixed-citation><mixed-citation xml:lang="en">Picό Y., Blasco C., Font G. Environmental and food applications of LC-MS-MS in pesticide-residue analysis: an overview. Mass Spectrom. Rev. 2004; 23(1): 45–85. https://doi.org/10.1002/mas.10071</mixed-citation></citation-alternatives></ref><ref id="cit8"><label>8</label><citation-alternatives><mixed-citation xml:lang="ru">Anastassiades M., Lehotay S.J., Stajnbaher D., Schenck F.J. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “Dispersive solid-phase extraction” for the determination of pesticide residues in produce. J. AOAC Int. 2003; 86(2): 412–31.</mixed-citation><mixed-citation xml:lang="en">Anastassiades M., Lehotay S.J., Stajnbaher D., Schenck F.J. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “Dispersive solid-phase extraction” for the determination of pesticide residues in produce. J. AOAC Int. 2003; 86(2): 412–31.</mixed-citation></citation-alternatives></ref><ref id="cit9"><label>9</label><citation-alternatives><mixed-citation xml:lang="ru">Anastassiades M., Mastovska K., Lehotay S.J. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides. J. Chromatogr. A. 2003; 1015(1-2): 163–84. https://doi.org/10.1016/s0021-9673(03)01208-1</mixed-citation><mixed-citation xml:lang="en">Anastassiades M., Mastovska K., Lehotay S.J. Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides. J. Chromatogr. A. 2003; 1015(1-2): 163–84. https://doi.org/10.1016/s0021-9673(03)01208-1</mixed-citation></citation-alternatives></ref><ref id="cit10"><label>10</label><citation-alternatives><mixed-citation xml:lang="ru">Lehotay S. J., de Kok A., Hiemstra M., van Bodegraven P. Validation of a fast and easy method for the determination of 229 pesticide residues in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J. AOAC Int. 2005; 88(2): 595.</mixed-citation><mixed-citation xml:lang="en">Lehotay S. J., de Kok A., Hiemstra M., van Bodegraven P. Validation of a fast and easy method for the determination of 229 pesticide residues in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J. AOAC Int. 2005; 88(2): 595.</mixed-citation></citation-alternatives></ref><ref id="cit11"><label>11</label><citation-alternatives><mixed-citation xml:lang="ru">European Committee for Standardization (CEN). Determination of pesticide residues using GC-MS(/MS) and/or LC-MS/MS following acetonitrile extraction/partitioning and cleanup by dispersive SPE – QuEChERS-method. CEN/TC 275 prEN 1556662; 2007. Available at: https://www.eurl-pesticides.eu/library/docs/cf/FP417%201%20%203%20%20udgave%20engelsk%20version.pdf</mixed-citation><mixed-citation xml:lang="en">European Committee for Standardization (CEN). Determination of pesticide residues using GC-MS(/MS) and/or LC-MS/MS following acetonitrile extraction/partitioning and cleanup by dispersive SPE – QuEChERS-method. CEN/TC 275 prEN 1556662; 2007. Available at: https://www.eurl-pesticides.eu/library/docs/cf/FP417%201%20%203%20%20udgave%20engelsk%20version.pdf</mixed-citation></citation-alternatives></ref><ref id="cit12"><label>12</label><citation-alternatives><mixed-citation xml:lang="ru">AOAC Official Method 2007.01. Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. Gas Chromatography/Mass Spectrometry and Liquid Chromatography/Tandem Mass Spectrometry First Action 2007. Available at: https://weber.hu/Downloads/SPE/QuEChERS/AOAC_2007_01.pdf</mixed-citation><mixed-citation xml:lang="en">AOAC Official Method 2007.01. Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. Gas Chromatography/Mass Spectrometry and Liquid Chromatography/Tandem Mass Spectrometry First Action 2007. Available at: https://weber.hu/Downloads/SPE/QuEChERS/AOAC_2007_01.pdf</mixed-citation></citation-alternatives></ref><ref id="cit13"><label>13</label><citation-alternatives><mixed-citation xml:lang="ru">Pang G.F., Liu Y.M., Fan C.L., Zhang J.J., Cao Y.Z., Li X.M., et al. Simultaneous determination of 405 pesticides residues in gran by accelerated solvent extraction then gas chromatography-mass spectrometry or liquid chromatograraphy-tandem mass spectrometry. Anal. Bioanal. Chem. 2006; 384(6): 1366–408. https://doi.org/10.1007/s00216-005-0237-9</mixed-citation><mixed-citation xml:lang="en">Pang G.F., Liu Y.M., Fan C.L., Zhang J.J., Cao Y.Z., Li X.M., et al. Simultaneous determination of 405 pesticides residues in gran by accelerated solvent extraction then gas chromatography-mass spectrometry or liquid chromatograraphy-tandem mass spectrometry. Anal. Bioanal. Chem. 2006; 384(6): 1366–408. https://doi.org/10.1007/s00216-005-0237-9</mixed-citation></citation-alternatives></ref><ref id="cit14"><label>14</label><citation-alternatives><mixed-citation xml:lang="ru">Kolberg D.I., Prestes О.D., Adaime M.B., Zenella R. Development of a fast multiresidues method for the determination of pesticides in dry samples (wheat grains, flour and bran) using QuEChERS based method and GC-MS. Food Chem. 2011; 125: 1436–42.</mixed-citation><mixed-citation xml:lang="en">Kolberg D.I., Prestes О.D., Adaime M.B., Zenella R. Development of a fast multiresidues method for the determination of pesticides in dry samples (wheat grains, flour and bran) using QuEChERS based method and GC-MS. Food Chem. 2011; 125: 1436–42.</mixed-citation></citation-alternatives></ref><ref id="cit15"><label>15</label><citation-alternatives><mixed-citation xml:lang="ru">Gonzalez-Curbelo M.A., Herrera-Herrera A.V., Ravelo-Perez L.V., Hernandes-Borges J. Sample-preparation methods for pesticide-residue analysis in cereals and derivatives. Trends Anal. Chem. 2012; 38: 32–51.</mixed-citation><mixed-citation xml:lang="en">Gonzalez-Curbelo M.A., Herrera-Herrera A.V., Ravelo-Perez L.V., Hernandes-Borges J. Sample-preparation methods for pesticide-residue analysis in cereals and derivatives. Trends Anal. Chem. 2012; 38: 32–51.</mixed-citation></citation-alternatives></ref><ref id="cit16"><label>16</label><citation-alternatives><mixed-citation xml:lang="ru">He Z., Wang L., Peng Y., Luo M., Wang W., Liu X. Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method. Food Chem. 2015; 169: 372–80. https://doi.org/10.1016/j.foodchem.2014.07.102</mixed-citation><mixed-citation xml:lang="en">He Z., Wang L., Peng Y., Luo M., Wang W., Liu X. Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method. Food Chem. 2015; 169: 372–80. https://doi.org/10.1016/j.foodchem.2014.07.102</mixed-citation></citation-alternatives></ref><ref id="cit17"><label>17</label><citation-alternatives><mixed-citation xml:lang="ru">Analytical Quality control and method validation procedures for pesticide residues analysis in food and feed. SANTE/12682/2019, Supersedes Document № SANTE/2017/11813. Implemented by 01/01/2020.</mixed-citation><mixed-citation xml:lang="en">Analytical Quality control and method validation procedures for pesticide residues analysis in food and feed. SANTE/12682/2019, Supersedes Document № SANTE/2017/11813. Implemented by 01/01/2020.</mixed-citation></citation-alternatives></ref><ref id="cit18"><label>18</label><citation-alternatives><mixed-citation xml:lang="ru">Analytical Method Report Analysis of Dithianon in Food of Plant Origin using acidified QuEChERS and LC-MS/MS. Available at: https://www.eurl-pesticides.eu/userfiles/file/EurlSRM/meth_Dithianon_EurlSRM.pdf</mixed-citation><mixed-citation xml:lang="en">Analytical Method Report Analysis of Dithianon in Food of Plant Origin using acidified QuEChERS and LC-MS/MS. Available at: https://www.eurl-pesticides.eu/userfiles/file/EurlSRM/meth_Dithianon_EurlSRM.pdf</mixed-citation></citation-alternatives></ref><ref id="cit19"><label>19</label><citation-alternatives><mixed-citation xml:lang="ru">Ракитский В.Н., Федорова Н.Е., Баюшева В.В., Егорченкова О.Е., Бондарева Л.Г. Определение 2,4-д в отдельных пищевых продуктах (молоко, яйца, печень, почки) хроматографическими методами. Токсикологический вестник. 2018; (1): 20–5. https://doi.org/10.36946/0869-7922-2018-1-20-25</mixed-citation><mixed-citation xml:lang="en">Rakitskiy V.N., Fedorova N.E., Bayusheva V.V., Egorchenkova O.E., Bondareva L.G. Determination of 2,4-d in some food products (milk, eggs, liver, kidneys) by chromatography methods. Toksikologicheskiy vestnik. 2018; (1): 20–5. https://doi.org/10.36946/0869-7922-2018-1-20-25 (in Russian)</mixed-citation></citation-alternatives></ref><ref id="cit20"><label>20</label><citation-alternatives><mixed-citation xml:lang="ru">Попова А.Ю., Ракитский В.Н., Федорова Н.Е., Липкина Л.И., Ларькина М.В., Соболев Д.Н. и др. Фипронил: химико-аналитическое обеспечение контроля безопасности пищевой продукции. Здоровье населения и среда обитания. 2018; 301(4): 10–4. https://doi.org/10.35627/2219-5238/2018-301-4-10-14</mixed-citation><mixed-citation xml:lang="en">Popova A.Yu., Rakitskiy V.N., Fedorova N.E., Lipkina L.I., Lar’kina M.V., Sobolev D.N., et al. Fipronil: chemical and analytical support for food safety control. Zdorov’e naseleniya i sreda obitaniya. 2018; 301(4): 10–4. https://doi.org/10.35627/2219-5238/2018-301-4-10-14 (in Russian)</mixed-citation></citation-alternatives></ref><ref id="cit21"><label>21</label><citation-alternatives><mixed-citation xml:lang="ru">Клисенко М.А., Калинина А.А., Новикова К.Ф., Хохолькова Г.А. Методы определения микроколичеств пестицидов в продуктах питания, кормах и внешней среде. Справочник. Том 1. М.: Колос; 1992.</mixed-citation><mixed-citation xml:lang="en">Klisenko M.A., Kalinina A.A., Novikova K.F., Khokhol’ko-va G.A. Methods for the Determination of Trace Amounts of Pesticides in Food, Feed and the Environment. Handbook. Volume 1 [Metody opredeleniya mikrokolichestv pestitsidov v produktakh pitaniya, kormakh i vneshney srede. Spravochnik. Tom 1]. Moscow: Kolos; 1992. (in Russian)</mixed-citation></citation-alternatives></ref></ref-list><fn-group><fn fn-type="conflict"><p>The authors declare that there are no conflicts of interest present.</p></fn></fn-group></back></article>
