Determination of 14 Anabolic Androgenic Steroids in Animal Derived Foods by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Jing; ZHANG Haichao; JIA Haitao; AI Lianfeng

doi:10.13386/j.issn1002-0306.2021120163

Volume 43 Issue 20

Oct. 2022

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Science and Technology of Food Industry > 2022 > 43(20): 291-299. > DOI: 10.13386/j.issn1002-0306.2021120163

WANG Jing, ZHANG Haichao, JIA Haitao, et al. Determination of 14 Anabolic Androgenic Steroids in Animal Derived Foods by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(20): 291−299. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021120163.

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Determination of 14 Anabolic Androgenic Steroids in Animal Derived Foods by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Technology Center of Shijiazhuang Customs, Shijiazhuang 050051, China

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Received Date: December 15, 2021
Available Online: August 17, 2022

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Abstract

Abstract

A method was developed for the determination of 14 anabolic androgenic steroids including trenbolone, boldenone and nandrolone in animal derived foods by liquid chromatography-tandem mass spectrometry. The samples were added to ammonium acetate buffer and enzymatic hydrolyzed by β-glucuronidase and arysulfatase. The hydrolyzates were extracted with 20 mL acetonitrile, and then 10 mL supernatant was degreased by 10 mL acetonitrile saturated hexane, purified with 50 mg C₁₈, 50 mg PSA and 300 mg neutral alumina powder including 300 mg MgSO₄. Then the analytes were separated by C₁₈ column with gradient elution using 0.1% formic acid and acetonitrile as the mobile phase, detected in positive multiple reaction monitoring (MRM) and quantified with matrix-matched external standards. The linear regression correlation coefficients for the compounds were all higher than 0.992 in the range from 0.1 to 10 ng/mL. The limits of detection and the limits of quantification were 0.3 and 1.0 μg/kg respectively. The recoveries at the addition levels of 1.0, 2.0 and 10 μg/kg were in the range of 75.7%~104.1%, with relative standard deviations (RSDs) of 3.60%~12.1%. This method had high effectivity, good reproducibility, simple operation and high efficiency, and could be used for the rapid determination needs of common anabolic androgenic steroids in foodborne stimulants in the Winter Olympic Games.
- liquid chromatography-tandem mass spectrometry,
- anabolic androgenic steroids,
- QuEChERS,
- animal derived foods

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[1]	房克艳, 赵超敏, 陈沁, 等. 超高效液相色谱-三重四级杆质谱法同时测定饲料中8种类固醇激素[J]. 食品工业科技,2019,40(13):172−179. [FANG K Y, ZHAO C M, CHEN Q, et al. Simultaneous determination of 8 steroid hormones in feed by ultra performance liquid chromatography-tandem mass spectrometry[J]. Science and Technology of Food Industry,2019,40(13):172−179.
[2]	段玉林, 陈砾岩, 宁方尧, 等. 肉制品中重金属及兽药残留现状研究[J]. 食品安全质量检测学报,2021,12(8):3008−3015. [DUAN Y L, CHEN L Y, NING F Y, et al. Study on the residual pollution of heavy metals and veterinary drugs in meat products[J]. Journal of Food Safety and Quality,2021,12(8):3008−3015.
[3]	DINH Q T, MUNOZ G, DUY S V, et al. Analysis of sulfonamides, fluoroquinolones, tetracyclines, triphenylmethane dyes and other veterinary drug residues in cultured and wild seafood sold in Montreal, Canada[J]. Journal of Food Composition and Analysis,2020,94:103630. doi: 10.1016/j.jfca.2020.103630
[4]	高洁, 陈达炜, 赵云峰. 通过式固相萃取-超高效液相色谱-串联质谱法快速测定猪肉中52种同化激素[J]. 中国卫生检验杂志,2018,28(12):1422−1425. [GAO J, CHEN D W, ZHAO Y F. Rapid determination of 52 anabolic hormones in pork by ultra high performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction[J]. Chin J Health Lab Tec,2018,28(12):1422−1425.
[5]	李凯华, 肖曼, 张玲, 等. 超高效液相色谱-串联质谱法测定鱼肉中多种雄性激素和孕激素[J]. 食品安全质量检测学报,2020,11(15):5068−5073. [LI K H, XIAO M, ZHANG L, et al. Determination of various androgens and progesterones in fish meat by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2020,11(15):5068−5073.
[6]	陈晓鹏, 顾采琴, 綦艳, 等. QuEChERS-UPLC-MS/MS同时测定牛奶和奶粉中42种类固醇激素[J]. 食品科学,2018,39(8):314−321. [CHEN X P, GU C Q, QI Y, et al. Simultaneous determination of 42 steroid hormones inmilk and milk power by QuEChERS combined with UPLC-MS/MS[J]. Food Science,2018,39(8):314−321. doi: 10.7506/spkx1002-6630-201808049
[7]	农业农村部, 中华人民共和国卫生部, 国家药品监督管理局. 中华人民共和国农业部公告第250号[S]. 北京: 中国农业出版社, 2019. Ministry of Agriculture and Rural Affairs Announcement, Ministry of Health of the People's Republic of China, State Administration for Market Regulation. Announcement No.250 of the ministry of agriculture of the people's republic of China[S]. Beijing: National Standards Press, 2019.
[8]	国家市场监督管理总局, 国家卫生健康委员会, 农业农村部. GB 31650-2019《食品安全国家标准食品中兽药最大残留限量》[S]. 北京: 中国农业出版社, 2020. State Administration for Market Regulation, National HMinistry of Agricultur and Rural Affairs Announcement, National Health Commission. GB 31650-2019 national food safety standard. maximum residue limits for veterinary drugs in foods[S]. Beijing: National Standards Press, 2020.
[9]	周秋玲, 娄婷婷, 王素英, 等. 动物源性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 gonadal hormone in animal derived food[J]. Food Research and Development,2018,39(9):183−189. doi: 10.3969/j.issn.1005-6521.2018.09.035
[10]	景晶, 王杉, 杨声, 等. 气相串接质谱联用法确证人尿中44种外源性蛋白同化激素[J]. 中国运动医学杂志,2020,39(6):476−481. [JING J, WANG S, YANG S, et al. Confirmation of forty-four exdogenous anabolic androgenic steroids in human urine using gas chromatography-mass spectrometry[J]. Chinese Journal of Sports Medicine,2020,39(6):476−481. doi: 10.3969/j.issn.1000-6710.2020.06.009
[11]	CHEN D, XU Q, LU Y P, et al. The QuEChERS method coupled with high-performance liquid chromatography-tandem mass spectrometry for the determination of diuretics in animal-derived foods[J]. Journal of Food Composition and Analysis,2021,101:1−7.
[12]	栗有志, 李艳美, 周均, 等. 分散微固相萃取-高效液相色谱-串联质谱法测定水样中3种氯霉素类和11种激素类药物残留[J]. 分析科学学报,2020,36(1):69−74. [LI Y Z, LI Y M, ZHOU Y, et al. Dispersive micro-solid phhase extraction combined with high performance liquid chromatography-tandem mass spectrometry for determination of 3 chloramphenicols and 11 hormones residue in water samples[J]. Journal of Analytical Science,2020,36(1):69−74.
[13]	刘学芝, 赵英莲, 马跃, 等. 超高效液相色谱-串联质谱法测定猪肉、鸡蛋、牛奶中9种食源性兴奋剂类药物残留[J]. 色谱,2022,40(2):148−155. [LIU X Z, ZHAO Y L, MA Y, et al. Determination of nine food-borne stimulant drug residues in pork, egg, and milk by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2022,40(2):148−155. doi: 10.3724/SP.J.1123.2021.04005
[14]	郭添荣, 吴文林, 张崟, 等. 基于UHPLC-Q/Orbitrap高分辨质谱多目标快速筛查鱼肉中30种蛋白同化激素及糖皮质激素[J]. 食品科学,2022,43(4):321−330. [GUO T R, WU W L, ZHANG Y, et al. Multi-objective rapid screening of 30 protein assimilation hormones and glucocorticoids infish by ultra-high performance liquid chromatography coupled to quadrupole/orbitrap high-resolution mass spectrometry[J]. Journal of Food Science,2022,43(4):321−330.
[15]	马俊美, 范素芳, 李强, 等. 超高效液相色谱-四极杆/飞行时间质谱检测猪肉和牛肉中30种食源性兴奋剂类药物残留[J]. 食品科学,2021,42(14):276−285. [MA J M, FAN S F, LI Q, et al. Determination of 30 foodborne stimulant drug residues in pork and beef using ultra-high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J]. Journal of Food Science,2021,42(14):276−285. doi: 10.7506/spkx1002-6630-20200624-329
[16]	孔祥一, 庄丽丽, 方恩华, 等. QuEChERS-同位素稀释-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物[J]. 色谱,2021,39(1):96−103. [KONG X Y, ZHUANG L L, FANG E H, et al. Determination of nine N-nitrosamines in animal derived foods by QuEChERS-isotope dilution combined with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2021,39(1):96−103. doi: 10.3724/SP.J.1123.2020.06010
[17]	程江闯, 胡启立, 吴海平. QuEChERS-超高效液相色谱-串联质谱法测定牛羊肉中36种瘦肉精残留量[J]. 食品安全质量检测学报,2020,11(23):8798−8808. [CHENG J C, HU Q L, WU H P. Determination of 36 clenbuterol residues in beef and mutton samples by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2020,11(23):8798−8808.
[18]	YE S B, HUANG Y, LIN D Y. QuEChERS sample pre-processing with UPLC-MS/MS: A method for detecting 19 quinolone-based veterinary drugs in goat's milk[J]. Food Chemistry,2022,373:131−466.
[19]	黄冬梅, 惠芸华, 沈晓盛, 等. HPLC-MS/MS测定河蟹中蛋白同化激素残留量[J]. 中国卫生检验杂志,2011,21(1):48−50. [HUANG D M, HUI Y H, SHEN X S, et al. Determination of protein anabolic steroids residues in river crab hy HPLC-MS/MS[J]. Chinese Journal of Health Laboratory Technology,2011,21(1):48−50.
[20]	戴唯, 李巧, 朱明, 等. QuEChERS-同位素内标-高效液相色谱-串联质谱法测定动物源性食品中植物生长调节剂类农药残留[J]. 色谱,2021,39(11):1213−1221. [DAI W, LI Q, ZHU M, et al. Determination of plant growth regulators in animal-derived foods using QuEChERS-isotope-labeled internal standards with high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2021,39(11):1213−1221. doi: 10.3724/SP.J.1123.2021.01029
[21]	王莉莉, 张楠, 刘平, 等. 通过式固相萃取结合QuEChERS前处理技术-液相色谱串联质谱法快速测定熟肉食品中4种β₂受体激动剂残留[J]. 食品安全质量检测学报,2021,12(9):3771−3776. [WANG L L, ZHANG N, LIU P, et al. Rapid determination of 4 kinds of β₂-agonist residues in cooked meat by pass-through solid phase extraction column combined with QuEChERS pretreatment technique-liquid chromatography tandem mass spectrometry[J]. Journal of Food Safety and Quality,2021,12(9):3771−3776.
[22]	XU X Y, ZHU B Q, LIU Z, et al. Development of a modified quick, easy, cheap, effective, rugged, and safe method based on melamine sponge for multi-residue analysis of veterinary drugs in milks by ultra-performance liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A,2021,1651:462333. doi: 10.1016/j.chroma.2021.462333
[23]	胡钰, 朱青青, 胡立刚, 等. 超高效液相色谱-串联质谱法同时测定土壤中30种抗生素[J]. 色谱,2021,39(8):878−888. [HU Y, ZHU Q Q, HU L G, et al. Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography,2021,39(8):878−888. doi: 10.3724/SP.J.1123.2021.02019
[24]	张再永, 马俊美, 李强, 等. 通过式固相萃取-超高效液相色谱-串联质谱法测定猪肉和牛肉中9种类固醇激素[J]. 肉类研究,2020,34(7):58−63. [ZHANG Z Y, MA J M, LI Q, et al. Determination of 9 steroid hormones in pork and beef samples by filtration solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Meat Research,2020,34(7):58−63. doi: 10.7506/rlyj1001-8123-20200429-109
[25]	卢巧梅, 童萍, 蔡惠坚, 等. 高效液相色谱-串联质谱法快速分析鱼肉中的类固醇激素残留[J]. 现代食品科技,2019,35(12):276−281,215. [LU Q M, TONG P, CAI H J, et al. Rapid analysis of steroid hormone residues in fish flesh by high performance liquid chromatography-tandem mass spectrometry[J]. Modern Food Science and Technology,2019,35(12):276−281,215.
[26]	张居舟, 李静. 在线固相萃取-同位素稀释/超高效液相色谱-串联质谱法测定蜂蜜中26种喹诺酮类化合物[J]. 分析测试学报,2011,40(10):1417−1424. [ZHANG J Z, LI J. Simultaneous determination of 26 quinolones in honey by UPLC-MS/MS with on-line solid-phase extraction and isotope dilution[J]. Journal of Instrumental Analysis,2011,40(10):1417−1424.
[27]	孙强, 李玉博, 温广月, 等. 分散固相萃取-超高效液相色谱-串联质谱法测定农产品中乙拌磷及其代谢物[J]. 色谱,2022,40(2):130−138. [SUN Q, LI Y B, WEN G Y, et al. Determination of disulfoton and its metabolites in agricultrral products by dispersive solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2022,40(2):130−138. doi: 10.3724/SP.J.1123.2021.04028
[28]	郑幸果, 赵珊, 李曦, 等. 超高效液相色谱-串联质谱法同时测定蜂蜜中4种抗病毒类药物残留[J]. 食品安全质量检测学报,2021,12(5):4110−4117. [ZHENG X G, ZHAO S, LI X, et al. Simultaneous determination of 4 kinds of antiviral drug residues in honey by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality,2021,12(5):4110−4117.
[29]	WANG C F, LI X W, YU F G, et al. Multi-class analysis of veterinary drugs in eggs using dispersive-solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry,2021,334:127−598.
[30]	XU X Y, ZHU B Q, LIU Z, et al. Simultaneous determination of eight microcystins in fish by PRiME pass-through cleanup and online solid phase extraction coupled to ultra high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography B,2019,1125:121−709.
[31]	杨明, 伊鋆, 胡筱静, 等. QuEChERS/高效液相色谱-串联质谱测定婴幼儿配方奶粉中14种β-受体激动剂[J]. 中国乳品工业,2019,47(11):52−56. [YANG Y, YINY, HU Y J, et al. Determination of 14 β-agonists in infant formulas using QuEChERS-High performance liquid chromatography-tandem mass spectrometry[J]. Dairy Industry,2019,47(11):52−56. doi: 10.3969/j.issn.1001-2230.2019.11.012
[32]	张虹艳, 邱国玉, 石晓峰, 等. 高效液相色谱-四极杆-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 illegally adulterated androgen drugs in health foods by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry[J]. Journal of Instrumental Analysis,2020,39(9):1085−1091. doi: 10.3969/j.issn.1004-4957.2020.09.004
[33]	魏丽丽, 薛霞, 武传香, 等. 混合型离子交换液相色谱-串联质谱法检测鸡蛋中10种氨基糖苷类药物残留[J]. 色谱,2021,39(12):1374−1381. [WEI L L, XUE X, WU C X, et al. Determination of ten aminoglycoside residues in eggs by mixed-mode ion exchange liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2021,39(12):1374−1381. doi: 10.3724/SP.J.1123.2021.02027