超高效液相色谱-串联质谱法检测鳗鲡肌肉中13种禁用β-受体激动剂残留
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摘要
建立了鳗鲡肌肉中13种禁用β-受体激动剂残留的UPLC-MS/MS检测方法。鳗鲡肌肉样品采用0. 2 mol/L乙酸铵溶液提取,β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,5%的三氯乙酸溶液沉淀蛋白,HLB固相萃取柱净化富集,目标化合物选用C_(18)色谱柱利用乙酸铵和乙腈梯度分离,UPLC-MS/MS在电喷雾离子源(ESI)正离子模式下以选择反应监测(SRM)模式定量分析。结果表明,13种β-受体激动剂在2. 5～100 ng/mL范围内线性关系良好,相关系数均大于0. 9938,在3个不同浓度(0. 5,1. 0,10μg/kg)水平下的基质加标,平均回收率在77. 0%～122. 0%之间,RSD为0. 59%～14%。方法检出限和定量限分别为0. 1μg/kg和0. 5μg/kg。方法适用于对鳗鲡中13种禁用β-受体激动剂残留的定性和定量分析。
A determination strategy of 13 banned β-agonists residues in eel muscle was established by ultra-high performance liquid chromatography triple-quadrupole mass spectrometry( UPLC-MS/MS).The samples were first pretreated by using β-glucoronidase/arylsulfatase to perform enzymatic hydrolysis,the product was then extracted by 0. 2 mol/L ammonium acetate solution. Subsequently,trichloroacetic acid( TCA) was added to remove proteins,and hydrophilic lipophilic balance( HLB)solid-phase extraction column cartridge was employed to purify and enrich the targets. The target compounds were separated through C_(18) chromatographic column,and quantified by UPLC-MS/MS which operated in positive selected reaction monitoring( SRM) mode. The method showed good linear in the range of 2. 5-100 ng/m L for the 13 β-agonists,with correlation coefficients( R~2) above0. 9938. The average recoveries at three spiked levels( 0. 5,1,10 μg/kg) ranged from 77. 0% to122. 0%,and the relative standard deviations( RSDs) ranged from 0. 59% to 14%. The limits of detection( LOD) and quantitation( LOQ) were 0. 1 μg/kg and 0. 5 μg/kg,respectively. This method was successfully applied to the simultaneous determination of 13 β-agonists residues in eel muscle.
A determination strategy of 13 banned β-agonists residues in eel muscle was established by ultra-high performance liquid chromatography triple-quadrupole mass spectrometry( UPLC-MS/MS).The samples were first pretreated by using β-glucoronidase/arylsulfatase to perform enzymatic hydrolysis,the product was then extracted by 0. 2 mol/L ammonium acetate solution. Subsequently,trichloroacetic acid( TCA) was added to remove proteins,and hydrophilic lipophilic balance( HLB)solid-phase extraction column cartridge was employed to purify and enrich the targets. The target compounds were separated through C_(18) chromatographic column,and quantified by UPLC-MS/MS which operated in positive selected reaction monitoring( SRM) mode. The method showed good linear in the range of 2. 5-100 ng/m L for the 13 β-agonists,with correlation coefficients( R~2) above0. 9938. The average recoveries at three spiked levels( 0. 5,1,10 μg/kg) ranged from 77. 0% to122. 0%,and the relative standard deviations( RSDs) ranged from 0. 59% to 14%. The limits of detection( LOD) and quantitation( LOQ) were 0. 1 μg/kg and 0. 5 μg/kg,respectively. This method was successfully applied to the simultaneous determination of 13 β-agonists residues in eel muscle.
引文
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[5] 176th Bulletin of the Ministry of Agriculture,List of substances prohibited in feed and animal drinking water[S]农业部第176号公告,禁止在饲料和动物饮用水中使用的物质名单
[6] 1519th Bulletin of the Ministry,List of substances prohibited in feed and animal drinking water[S]农业部第1519号公告,禁止在饲料和动物饮用水中使用的物质名单
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[8] Commission regulation(EU)No 37/2010,On pharmacologically active substances and their classification regarding maximum residue in foodstuffs of animal origin
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[10] GB/T 22950-2008,Determination of 12β-agonists residues in fugu,eel and baked eel-LC-MS-MS method GB/T 22950-2008,河豚鱼、鳗鱼和烤鳗中12种β-兴奋剂残留量的测定液相色谱-串联质谱法
[11] Luo H T,Huang X L,Wu H Q,Zhu Z X,Huang F,Lin X S,Zhang Q Y,Ma Y F. Chinese J Chromatogr,2016,34(5):481罗辉泰,黄晓兰,吴惠勤,朱志鑫,黄芳,林晓珊,张秋炎,马叶芬.色谱,2016,34(5):481
[12] Han W Q,Wu C S,Wu Y L,Dong H,Wang L,Wang B,Xian Y P,Luo H Y. Chinese J Anal Chem,2016,44(2):289韩婉清,吴楚森,吴玉銮,董浩,王莉,王斌,冼燕萍,罗海燕.分析化学,2016,44(2):289
[13] GB/T 22286-2008,Determination ofβ-agonists residues in food stuff of animalorigin-Liquid chromatography with tandemmass spectrometric method GB/T 22286-2008,动物源性食品中多种β-受体激动剂残留量的测定液相色谱串联质谱法
[14] Xiong L,Gao Y Q,Li W H,Guo T F,Yang X L. Food Sci Biotechnol,2015,24(5):1629
[15] Sung I K,Park S J,Kang K,Kim M Y,Cho S B. Korean J Food Sci An,2015,35(1):121
[16] Caban M,Migowska N,Stepnowski P,Kwiatkowski M,Kumirska J. J Chromatogr A,2010,1258:117
[2] LI Y,Su X O,Wang R G,Wang P L,Zhang W,Cheng J. Chinese J Anal Chem.,2013,41(6):899李阳,苏晓鸥,王瑞国,王培龙,张维护,程劼.分析化学,2013,41(6):899
[3] Guo C C,Shi F,Gong L P,Tan H J,Hu D F,Zhang J L. J Pharm Biomed Anal.,2015,107:526
[4] ZhangZ H,Yan H,Cui F Y,Yun H,Chang X H,Li J H,Liu X,Yang L J,Hu Q R. Food Anal Methods,2016,9(4):915
[5] 176th Bulletin of the Ministry of Agriculture,List of substances prohibited in feed and animal drinking water[S]农业部第176号公告,禁止在饲料和动物饮用水中使用的物质名单
[6] 1519th Bulletin of the Ministry,List of substances prohibited in feed and animal drinking water[S]农业部第1519号公告,禁止在饲料和动物饮用水中使用的物质名单
[7] Yan F,Zhang F. Feed Ind,2013,34(15):61袁飞,张峰.饲料工业,2013,34(15):61
[8] Commission regulation(EU)No 37/2010,On pharmacologically active substances and their classification regarding maximum residue in foodstuffs of animal origin
[9] Codex Alimentarius Commission,Maximum residue limits(MRL)risk management recommendations(RMRs)for residues of veterinary drugs in foods
[10] GB/T 22950-2008,Determination of 12β-agonists residues in fugu,eel and baked eel-LC-MS-MS method GB/T 22950-2008,河豚鱼、鳗鱼和烤鳗中12种β-兴奋剂残留量的测定液相色谱-串联质谱法
[11] Luo H T,Huang X L,Wu H Q,Zhu Z X,Huang F,Lin X S,Zhang Q Y,Ma Y F. Chinese J Chromatogr,2016,34(5):481罗辉泰,黄晓兰,吴惠勤,朱志鑫,黄芳,林晓珊,张秋炎,马叶芬.色谱,2016,34(5):481
[12] Han W Q,Wu C S,Wu Y L,Dong H,Wang L,Wang B,Xian Y P,Luo H Y. Chinese J Anal Chem,2016,44(2):289韩婉清,吴楚森,吴玉銮,董浩,王莉,王斌,冼燕萍,罗海燕.分析化学,2016,44(2):289
[13] GB/T 22286-2008,Determination ofβ-agonists residues in food stuff of animalorigin-Liquid chromatography with tandemmass spectrometric method GB/T 22286-2008,动物源性食品中多种β-受体激动剂残留量的测定液相色谱串联质谱法
[14] Xiong L,Gao Y Q,Li W H,Guo T F,Yang X L. Food Sci Biotechnol,2015,24(5):1629
[15] Sung I K,Park S J,Kang K,Kim M Y,Cho S B. Korean J Food Sci An,2015,35(1):121
[16] Caban M,Migowska N,Stepnowski P,Kwiatkowski M,Kumirska J. J Chromatogr A,2010,1258:117