Determination of residual amounts of beta-adrenostimulants in muscle tissue and liver by dispersion purification chromatography-mass spectrometry

Мұқаба

Дәйексөз келтіру

Толық мәтін

Ашық рұқсат Ашық рұқсат
Рұқсат жабық Рұқсат берілді
Рұқсат жабық Рұқсат ақылы немесе тек жазылушылар үшін

Аннотация

A selective technique for the determination of 20 beta-adrenostimulants in muscle tissue and liver by chromatography-mass spectrometry has been developed. The limit of quantitative determination of the technique is 0.1-0.25 (0.5) µg/kg (depending on the compound to be determined). The technique is based on hydrolysis of research objects followed by extraction of the determined compounds with acetic acid acetonitrile, obtaining the organic fraction by salting, its purification on aluminum oxide layer and dispersive purification with C18, further purification by liquid-liquid extraction with hexane. Data on promising ion-transitions of some determined compounds are given; detection parameters of bambuterol, formoterol, phenylethanolamine A are established. Data on optimization of hydrolysis, extraction and purification of extracts are given. Information on stage-by-stage losses of the determined compounds is given; data on the analysis of reference material are obtained. The validation of the developed method shows that the relative expanded uncertainty ranges from 7 to 24 %.

Толық мәтін

Рұқсат жабық

Авторлар туралы

A. Sorokin

All-Russian State Center for Quality and Standardization of Drugs for Animals and Feeds (FGBU VGNKI)

Хат алмасуға жауапты Автор.
Email: alex_sorokin@list.ru
Ресей, Moscow

Әдебиет тізімі

  1. Xiaomei W., Tongling L., Beloglazova N., Luo P., Qu J., Jiang W. Development of a competitive indirect enzyme-linked immunosorbent assay for screening phenylethanolamine A residues in pork samples // Food Anal. Methods. 2016. № 9. P. 3099.
  2. Li C., Li J., Jiang W., Zhang S., Shen J., Wen K., Wang Z. Development and application of a gel-based immunoassay for the rapid screening of salbutamol and ractopamine residues in pork // J. Agric. Food Chem. 2015. V. 63. № 48. P. 10556.
  3. Cooper J., Delahaut P., Fodey T.L., Elliott C.T. Development of a rapid screening test for veterinary sedatives and the beta-blocker carazolol in porcine kidney by ELISA // Analyst. 2004. V. 129. № 2. P. 169.
  4. Zhang Y., Wang F., Fang L., Wang S., Fang G. Rapid determination of ractopamine residues in edible animal products by enzyme-linked immunosorbent assay: Development and investigation of matrix effects // J. Biomed Biotechnol. 2009. P. 579175.
  5. Лемясева С.В. Определение стимулятора роста рактопамина в мясе индейки методом иммуноферментного анализа // Проблемы ветеринарной санитарии, гигиены и экологии. 2013. № 2(10). С. 12.
  6. Никитенко А.Н. Разработка методики определения содержания бета-адреностимуляторов в мясной и молочной продукции методом иммуноферментного анализа // Труды БГТУ. 2016. № 4. С. 195.
  7. Damasceno L., Ventura R., Cardoso J., Segura J. Diagnostic evidence for the presence of beta-agonists using two consecutive derivatization procedures and gas chromatography-mass spectrometric analysis // J. Chromatogr. B: Anal. Technol. Biomed. Life Sci. 2002. V. 780. № 1. P. 61.
  8. Caban M., Stepnowski P., Kwiatkowski M., Migowska N., Kumirska J. Determination of β-blockers and β-agonists using gas chromatography and gas chromatography-mass spectrometry – A comparative study of the derivatization step // J. Chromatogr. A. 2011. V. 1218. № 44. P. 8110.
  9. Damasceno L., Ventura R., Ortuño J., Segura J. Derivatization procedures for the detection of beta(2)-agonists by gas chromatographic/mass spectrometric analysis // J. Mass Spectrom. 2000. V. 35. № 11. P. 1285.
  10. Cheng J., Wang S., Su XO. Simultaneous identification and quantification of 20 β-receptor agonists in feed using gas chromatography-tandem mass spectrometry // PLoS One. 2013. V. 8. № 10. Article e76400.
  11. ГОСТ 31982-2012. Продукты пищевые, корма, продовольственное сырье. Метод определения содержания бета-адреностимуляторов с помощью газовой хроматографии с масс-спектрометрическим детектором. М.: Стандартинформ, 2020. 20 с.
  12. ГОСТ 33486-2015. Продукты пищевые, комбикорма, объекты биологические животного происхождения. Метод определения содержания бета-адреностимуляторов с помощью высокоэффективной жидкостной хроматографии с масс-спектрометрическим детектированием. М.: Стандартинформ, 2020. 25 с.
  13. Śniegocki T., Sell B., Posyniak A. Analysis of β-agonists in different biological matrices by liquid chromatography-tandem mass spectrometry // J. Vet Res. 2021. V. 65. № 4. P. 469.
  14. Yan Y., Ning J., Cheng X., Lv Q., Teng S., Wang W. Rapid and high-throughput determination of sixteen β-agonists in livestock meat using one-step solid-phase extraction coupled with UHPLC-MS/MS // Foods. 2022. V. 12. № 1. P. 76.
  15. Wu Y., Miao H., Fan S., Zhao Y.F. Determination of 23 β2-agonists and 5 β-blockers in animal muscle by high performance liquid chromatography-linear ion trap mass spectrometry // Sci. China Chem. 2010. V. 53. P. 832.
  16. Guo P., Wan J., Zhan C., Zhu C., Jiang W., Ke Y., Ding S., Wang D. A simplified sample pretreatment for the rapid determination of 22 β-agonist residues in swine muscle and liver tissues by ultra-high-performance liquid chromatography tandem mass spectrometry // J. Chromatogr. B: Anal. Technol. Biomed. Life Sci. 2018. V. 1096. P. 122.
  17. Xiong L., Gao Y.Q., Li W.H., Guo T., Yang X.L. A method for multiple identification of four β2-Agonists in goat muscle and beef muscle meats using LC-MS/MS based on deproteinization by adjusting pH and SPE for sample cleanup // Food Sci. Biotechnol. 2015. V. 24. P. 1629.
  18. Yanfei T., Fangwei Z., Dongmei C., Shuyu X., Pan Y., Xu W., Zhenli L., Dapeng P., Zonghui Y. Evaluation of matrix solid-phase dispersion extraction for 11 β-agonists in swine feed by liquid chromatography with electrospray ionization tandem mass spectrometry // J. Sep. Sci. 2014. V. 37. № 18. P. 2574.
  19. Ling Z., Yujie W., Yongfeng Z., Lihua L., Yanjuan M. Simultaneous determination of 18 β-agonist residues in feed using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry // Se Pu. 2014. V. 32. № 8. P. 867.
  20. Hongcheng L., Tao L., Xianglei C., Ning L., Luxiang W., Qiwan L. Simultaneous determination of anabolic steroids and β-agonists in milk by QuEChERS and ultra high performance liquid chromatography tandem mass spectrometry // J. Chromatogr. B: Anal. Technol. Biomed. Life Sci. 2017. V. 1043. P. 176.
  21. Lin Y.P., Lee Y.L., Hung C.Y., Huang W.J., Lin S.C. Determination of multiresidue analysis of β-agonists in muscle and viscera using liquid chromatograph/tandem mass spectrometry with quick, easy, cheap, effective, rugged, and safe methodologies // J. Food Drug Anal. 2017. V. 25. № 2. P. 275.
  22. Zhang L., Jia Q., Liao G., Qian Y., Qiu J. A fast method for the simultaneous analysis of 26 beta-agonists in swine muscle with a multi-functional filter by Ultra-High performance liquid chromatography-tandem mass spectrometry // Separations. 2022. V. 9. № 5. P. 121.

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2. Fig. 1. Examples of mass chromatograms of formoterol, phenylethanolamine A, and bambuterol in a liver sample at the limit of quantification.

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3. Fig. 2. Mass chromatograms of beta-agonists in a reference liver sample (a) without hydrolysis, (b) with hydrolysis using 30 µL of enzyme.

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4. Fig. 3. Comparison of peak areas of target compounds using different extractants. X-1 – 1% acetic acid in acetonitrile, X-3 – 1% ammonia solution in acetonitrile, X-4 – 0.1% acetic acid in acetonitrile.

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5. Fig. 4. Comparison of peak areas of target compounds during phase separation by salting out with different salts. S-2 – sodium sulfate and sodium chloride, S-3 – ammonium sulfate, S-4 – ammonium sulfate and sodium chloride.

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6. Fig. 5. Comparison of peak areas of target compounds using different purification methods. C-1 – 2 g of aluminum oxide and 1 g of C18, C-2 – 1 g of C18, C-3 – 2 g of aluminum oxide and 0.5 g of C18.

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7. Fig. 6. Comparison of average intensities of daughter ions of beta-agonists. CM-1 – multifunctional filter, CM-2 – separate extract purification.

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8. Fig. 7. Mass chromatograms of GM-clenbuterol and fenoterol at different spiking levels using multifunctional filter (CM-1) and separate extract purification (CM-2).

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9. Scheme 1. Structural formulas of formoterol (a), phenylethanolamine A (b), bambuterol (c).

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