Study and Application on the Method of Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry for Rapid Screening of Multiple Hormone Residues in Animal Tissues

YE Leihai; YE Jiaming; QIU Juntao; ZHONG Shihuan; HUANG Nan; ZHAN Yuecheng; HE Bin; WANG Qingling

doi:10.13386/j.issn1002-0306.2021030099

Volume 42 Issue 24

Dec. 2021

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Science and Technology of Food Industry > 2021 > 42(24): 229-238. > DOI: 10.13386/j.issn1002-0306.2021030099

YE Leihai, YE Jiaming, QIU Juntao, et al. Study and Application on the Method of Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry for Rapid Screening of Multiple Hormone Residues in Animal Tissues[J]. Science and Technology of Food Industry, 2021, 42(24): 229−238. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021030099.

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Study and Application on the Method of Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry for Rapid Screening of Multiple Hormone Residues in Animal Tissues

1.
Zhejiang Gongzheng Testing Center Company, Hangzhou 310009, China
2.
Zanyu Technology Group Corporation, Hangzhou 310009, China

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Received Date: March 08, 2021
Available Online: October 13, 2021

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Abstract

A method for rapid screening of 32 hormone residues in animal tissues by liquid chromatography quadrupole time of flight mass spectrometry (LC-Q-TOF/MS) was established. Samples were extracted by acetonitrile and ethyl acetate and extracted was purified by enhanced lipid removal adsorbent (EMR). After salting out, extract were further purified by PSA and functionalized polystyrene/two vinyl benzene (PEP-2), with 0.1% formic acid water-0.1% formic acid was used as mobile phase for gradient elution, in Eclipse plus-C₁₈ (3.0 mm×100 mm, 1.8 μm) column on the chromatographic column separation. The mass spectrum data were collected in Q-TOF/MS positive ion full scan mode. The retention time, accurate molecular mass number, isotopic abundance ratio and secondary characteristic fragment ions were used for qualitative analysis, and the excimer ion peak area was used for quantitative analysis. The results showed that all the drugs had good linearity in their respective concentration range, and the correlation coefficients was greater than 0.995. The average recoveries ranged from 70.3% to 116.2% at the addition levels of 10, 50 and 100 μg/kg. The relative standard deviation was 0.87% to 8.97%. The limit of detection was 1～10 μg/kg and the limit of quantification was 3～30 μg/kg. By constructing a first-order accurate mass database and a second-order spectral library, combine with retention time, accurate molecular mass number, isotope abundance ratio and secondary characteristic fragment ions, the method could achieve rapid screening and confirmation of target compounds. It had the advantages of simply, rapidity, high sensitivity, high selectivity and good precision, and was suitable for rapid screening and quantitative determination of multiple hormones in animal tissues.

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[1]	LITWACK G. Chapter16-steroid hormones[M]. Boston: Academic Press, 2018: 467−506.
[2]	BARRBARA S R, DARINA L, KATERINA U, et al. Multiclass analytical method for the determination of natural/synthetic steroid hormones, phytoestrogens, and mycoestrogens in milk and yogurt[J]. Analytical and Bioanalytical Chemistry,2017,409(18):4467−4477. doi: 10.1007/s00216-017-0391-x
[3]	李宁, 林小莉, 董艳峰, 等. 饲料中非法添加激素类药物检测方法研究[J]. 黑龙江畜牧兽医,2016(8):166−168. [LI N, LIN X L, DONG Y F, et al. Study on the detection method of hormone drugs illegally added in feed[J]. Heilongjiang Animal Husbandry and Veterinary Medicine,2016(8):166−168.
[4]	European Union. Commision regulation (EU) No 37/2010 of 22 December 2009[S].
[5]	中华人民共和国农业部. 中华人民共和国农业部公告第250 号公告[EB/OL].2019-12-27. Ministry of agriculture of the people’s Republic of China. Announcement No. 250 of the Ministry of agriculture of the people’s Republic of China[EB/OL]. 2019-12-27.
[6]	国家市场监督管理总局. 食品安全国家标准 GB 31650-2019 食品中兽药最大残留限量[S]北京: 中国标准出版社, 2019. State Administration of market supervision. National food safety standard GB 31650-2019 Maximum residue limits of veterinary drugs in food [S] Beijing: China Standards Press, 2019.
[7]	SCARTH J P, KAY J, TEALE P, et al. A review of analytical strategies for the detection of ‘endogenous’ steroid abuse in food production[J]. Drug Testing & Analysis,2012,4(S1):40−49.
[8]	卢杰, 冯晓梅, 隋晓, 等. 亚临界1, 1, 1, 2-四氟乙烷萃取-气相色谱-质谱法测定鱼肉中6种性激素残留[J]. 分析化学, 2013, 41(10): 1487−1492. LU J, FENG X M, SUI X, et al. Determination of six sex hormone residues in fish by GC-MS with subcritical 1, 1, 1, 2-tetrafluoroethane extraction[J]. Analytical Chemistry, 2013, 41(10): 1487−1492.
[9]	欧贝丽, 赵佳丽, 邹燕, 等. HPLC同时测定中成药及保健品中添加的16种糖皮质激素[J]. 中国现代应用药学,2016,33(9):1178−1182. [OU B L, ZHAO J L, ZOU Y, et al. Simultaneous determination of 16 glucocorticoids in Chinese patent medicines and health care products by HPLC[J]. Chinese Journal of Modern Applied Pharmacy,2016,33(9):1178−1182.
[10]	FRENCH D. Advances in bioanalytical techniques to measure steroid hormones in serum[J]. Bioanalysis,2016,8(11):1203−1219. doi: 10.4155/bio-2015-0025
[11]	王飞, 宓捷波, 葛含光, 等. 超高压液相色谱串联质谱法快速测定牛肉、牛肾中3种甾类同化激素药物残留量[J]. 质谱学报,2019,40(1):83−89. [WANG F, MI J B, GE H G, et al. Rapid determination of three steroid assimilating hormone residues in beef and kidney by ultra high pressure liquid chromatography tandem mass spectrometry[J]. Acta Mass Spectrometry,2019,40(1):83−89. doi: 10.7538/zpxb.2018.0081
[12]	RAYCO G A, ZORAIDA S F, JOSÉ J S R. Determination of steroid hormones in fish tissues by microwave-assisted extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry[J]. Food Chemistry,2017,237:1012−1020. doi: 10.1016/j.foodchem.2017.06.065
[13]	周秋玲, 娄婷婷, 王素英, 等. 动物源食品中性激素检测方法的比较分析[J]. 食品研究与开发,2018,39(9):183−189. [ZHOU Q L, LOU T T, WANG S Y, et al. Comparative analysis of detection methods of sexual hormones in animal-derived foods[J]. Food Research and Development,2018,39(9):183−189. doi: 10.3969/j.issn.1005-6521.2018.09.035
[14]	MICKAEL D, CAROLINE W, EMMANUELLE B, et al. Supercritical fluid chromatography applied to the highly selective isolation of urinary steroid hormones prior to GC/MS analysis[J]. Journal of Chromatography B,2018,1086:97−104. doi: 10.1016/j.jchromb.2018.04.024
[15]	张虹艳, 邱国玉, 石晓峰, 等. 高效液相色谱-四级杆-飞行时间质谱法快速筛查保健食品中10种雄性激素类非法添加物[J]. 分析测试学报,2020,39(9):1085−1091. [ZHANG H Y, QIU G Y, SHI X F, et al. Rapid screening of 10 kinds of illegal androgen additives in health food by high performance liquid chromatography quadrupole time of flight mass spectrometry[J]. Acta Analytica Sinica,2020,39(9):1085−1091. doi: 10.3969/j.issn.1004-4957.2020.09.004
[16]	恭松松, 张婧, 严凤, 等. 超高效液相色谱一四极杆飞行时间质谱快速筛查与确证生鲜牛乳中80种抗生素和激素[J]. 分析测试学报,2019,38(1):22−30. [GONG S S, ZHANG J, YAN F, et al. Rapid screening and confirmation of 80 antibiotics and hormones in fresh milk by ultra performance liquid chromatography quadrupole time of flight mass spectrometry[J]. Acta Analytica Sinica,2019,38(1):22−30. doi: 10.3969/j.issn.1004-4957.2019.01.003
[17]	胡争艳, 王天娇, 王丽媛, 等. 磁性多壁碳纳米管分散固相萃取-超高效液相色谱-串联质谱法同时测定婴幼儿配方奶粉中14种性激素残留[J]. 中国卫生检验杂志,2018,28(6):641−649. [HU Z Y, WANG T J, WANG L Y, et al. Simultaneous determination of 14 sex hormones residues in infant formula milk powder by magnetic multi-walled carbon nanotubes dispersion solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Health Laboratory Technology,2018,28(6):641−649.
[18]	曹江平, 邸宏伟, 周继梅, 等. 分散液液微萃取技术的研究进展[J]. 分析测试学报,2016,35(7):913−921. [CAO J P, DI H W, ZHOU J M, et al. Research progress of dispersed liquid-liquid microextraction technology[J]. Journal of Analytical Testing,2016,35(7):913−921. doi: 10.3969/j.issn.1004-4957.2016.07.025
[19]	蓝航镇. 新型固相微萃取涂层的研制及其应用于食品中雌激素残留的分析研究[D]. 宁波: 宁波大学, 2015. LAN H Z. Development of a new solid phase microextraction coating and its application in the analysis of estrogen residues in food [D]. Ningbo: Ningbo University, 2015.
[20]	李涛, 杨潇, 孙桂芳, 等. QuEChERS-UPLC-Q/Orbitrap MS 法快速测定草鱼中14 种糖皮质激素类药物残留[J]. 食品与机械,2019,35(12):101−104. [LI T, YANG X, SUN G F, et al. Rapid determination of 14 glucocorticoids residues in grass carp by quechers-uplc-q/Orbitrap MS[J]. Food and Machinery,2019,35(12):101−104.
[21]	卢杰. 亚临界R134a萃取技术在水产品性激素多残留分析中的应用研究[D]. 青岛: 中国海洋大学, 2014. LU J. Application of subcritical R134a extraction technology in multi-residue analysis of sex hormones in aquatic products [D]. Qingdao: Ocean University of China, 2014.
[22]	MRTA Z, BOB L Y B, FEKETE J, et al. Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system[J]. Journal of Pharmaceutical and Biomedical Analysis,2018,150:258−267. doi: 10.1016/j.jpba.2017.12.014
[23]	TAN X T, LI Z M, DENG L G, et al. Analysis of 13 kinds of steroid hormones in raw milk using modified QuEChERS method combined with UPLC-QTOF-MS[J]. Journal of Integrative Agriculture,2016,15(9):2163−2174. doi: 10.1016/S2095-3119(16)61386-2
[24]	赵子佳, 张宇, 孙佳明, 等. 动物源性食品中残留前处理技术及检测方法研究进展[J]. 吉林中医药,2017,37(1):55−57. [ZHAO Z J, ZHANG Y, SUN J M, et al. Research progress on pretreatment technology and detection methods of residues in animal-derived foods[J]. Jilin Traditional Chinese Medicine,2017,37(1):55−57.
[25]	李诗言, 王扬, 周凡, 等. 新型QuEChERS方法结合高效液相色谱串联飞行时间质谱法快速测定鱼肉中14种激素[J]. 中国渔业质量与标准,2016,6(5):52−59. [LI S Y, WANG Y, ZHOU F, et al. Rapid determination of 14 hormones in fish by new QuEChERS method combined with high performance liquid chromatography tandem time of flight mass spectrometry[J]. China Fisheries Quality and Standard,2016,6(5):52−59.
[26]	刘芸, 丁涛, 廖雪晴, 等. 高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法快速筛查中成药和保健食品中非法添加的42 种化学药物[J]. 分析化学,2016,44(3):423−429. [LIU Y, DING T, LIAO X Q, et al. Rapid screening of 42 kinds of illegally added chemicals in Chinese patent medicine and health food by high performance liquid chromatography quadrupole/electrostatic field orbital trap high resolution mass spectrometry[J]. Analytical Chemistry,2016,44(3):423−429. doi: 10.11895/j.issn.0253-3820.150726
[27]	陈晶燕, 陈万勤, 刘柱, 等. HPLC-MS/MS法同时测定鸡肉中40种糖皮质激素和9种非甾体抗炎药物残留[J]. 质谱学报,2019,40(2):123−130. [CHEN J Y, CHEN W Q, LIU Z, et al. Simultaneous determination of 40 glucocorticoids and 9 nonsteroidal anti-inflammatory drug residues in chicken by HPLC-MS/MS[J]. Journal of Mass Spectrometry,2019,40(2):123−130. doi: 10.7538/zpxb.2018.0022
[28]	BLASCO C , POUCKE C V , PETEGHEM C V. Analysis of meat samples for anabolic steroids residues by liquid chromatography/tandem mass spectrometry[J]. Journal of Chromatography A,2007,1154(1/2):230.
[29]	李佩佩, 郭远明, 张小军, 等. 高效液相色谱-串联质谱法测定动物源食品中同化激素的研究进展[J]. 理化检验(化学分册),2014(11):1476−1480. [LI P P, GUO Y M, ZHANG X J, et al. Research progress in determination of assimilating hormones in animal derived food by high performance liquid chromatography tandem mass spectrometry[J]. Physical and chemical examination (Chemistry),2014(11):1476−1480.
[30]	潘虹. 超高效液相色谱-串联四极杆飞行时间质谱法测定人体尿液中14种内源性甾体激素含量[J]. 理化检验-化学分册,2017,53(7):832−837. [PAN H. UPLC-QTOF/MS determination of 14 endogenous steroids in human urine[J]. Part B: Chemical Analysis,2017,53(7):832−837.

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Science and Technology of Food Industry

Study and Application on the Method of Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry for Rapid Screening of Multiple Hormone Residues in Animal Tissues

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