高效液相色谱-串联质谱法检测鲜冻肉中违禁注水药物
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摘要
建立鲜冻肉中同时检测阿托品、利多卡因、普鲁卡因、山莨菪碱、东莨菪碱、沙丁胺醇6种违禁注水药物残留的高效液相色谱-串联质谱法。样品经磷酸盐缓冲液提取,HLB固相萃取小柱净化,采用多反应监测模式检测,外标法定量分析。结果表明:6种药物在0.25~50 ng/mL范围内线性关系良好,线性相关系数均大于0.99,检出限和定量限分别为0.5μg/kg和2.0μg/kg;回收率在78.07%~96.76%之间,精密度的相对标准偏差在0.4%~2.1%之间(n=6)。该方法前处理简单、快速、准确、灵敏,可以满足实际检测分析的需要。
An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of six illegal water-retaining drugs,atropine,lidocaine,procaine,anisodamine,scopolamine and salbutamol,in frozen meat.The samples were extracted with phosphate buffer,and the extract was cleaned up on an HLB cartridge.The analytes were detected in the multiple reaction monitoring mode and quantified by the external standard method.The results indicated that good linearity over the concentration range of 0.25–50 ng/mL was observed for all analytes with correlation coefficients greater than 0.99.The limits of detection(LOD) and quantification(LOQ) were 0.5 and 2.0 μg/kg,respectively.The average recoveries of the six drugs ranged from 78.07% to 96.76% with relative standard deviations(RSDs) of 0.4%–2.1%(n = 6).The method is sensitive,simple,rapid and accurate and can meet the requirements of practical analysis.
An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of six illegal water-retaining drugs,atropine,lidocaine,procaine,anisodamine,scopolamine and salbutamol,in frozen meat.The samples were extracted with phosphate buffer,and the extract was cleaned up on an HLB cartridge.The analytes were detected in the multiple reaction monitoring mode and quantified by the external standard method.The results indicated that good linearity over the concentration range of 0.25–50 ng/mL was observed for all analytes with correlation coefficients greater than 0.99.The limits of detection(LOD) and quantification(LOQ) were 0.5 and 2.0 μg/kg,respectively.The average recoveries of the six drugs ranged from 78.07% to 96.76% with relative standard deviations(RSDs) of 0.4%–2.1%(n = 6).The method is sensitive,simple,rapid and accurate and can meet the requirements of practical analysis.
引文
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[19]毛谊平,任荣军,吴高芬.苍术中非法添加硫酸阿托品及氢溴酸东莨菪碱的检测方法[J].中国药业,2010,19(14):47-49.DOI:10.3969/j.issn.1006-4931.2010.14.031.
[20]韦寿莲,莫金垣,郑一宁.一种简单快速的高效毛细管电泳分离检测山莨菪碱和多沙唑嗪的方法[J].分析化学,2003,31(2):225-228.
[21]AZIZI S N,CHAICHI M J,SHAKERI P,et al.Determination of atropine using Mn-doped Zn S quantum dots as novel luminescent sensitizers[J].Journal of Luminescence,2013,144(12):34-40.DOI:10.1016/j.jlumin.2013.05.054.
[22]CHEN H P,SAEZ J M,GONZALEZ R R,et al.Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified Qu ECh ERs and liquid chromatography tandam mass spectrometry[J].Food Chemistry,2017,218:173-180.DOI:10.1016/j.foodchem.2016.09.075.
[23]SRAMSKA P,MACIEJKA A,TOPOLEWSKA A,et al.Isolation of atropine and scopolamine from plant material using liquid-liquid extraction and extrelut columns[J].Journal of Chromatography B,2017,1043:202-208.DOI:10.1016/j.jchromb.2016.09.003.
[24]SAEZ J M,GONZALEZ R R,FRENICH A G,et al.Enantiomeric determination and evaluation of the racemization process of atropine in Solanaceae seeds and contaminated samples by high performance liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A,2016,1474:79-84.DOI:10.1016/j.chroma.2016.10.047.
[25]KOZELJ G,PERHARIC L,STANOVNIK L,et al.Simple validated LC-MS/MS method for the determination of atropine and scopolamine in plasma for clinical and forensic toxicological purposes[J].Journal of Pharmaceutical and Biomedical Analysis,2014,96:197-206.DOI:10.1016/j.jpba.2014.03.037.
[26]刘谷歌,潘颖,陈桂良.猪血浆中阿托品含量的毛细管气相色谱测定[J].中国医药工业杂志,2003,34(5):132-139.DOI:10.3969/j.issn.1001-8255.2003.05.014.
[27]胡兴娟,吴宁鹏,董瑞静,等.UPLC-MS/MS测定4种兽药制剂中非法添加阿托品的方法研究[J].中国兽药杂志,2014,48(7):49-52.
[28]陈怀侠,杜鹏,韩凤梅,等.液相色谱-串联质谱法鉴定大鼠血浆中的阿托品及其代谢物[J].药物分析杂志,2006,26(10):1369-1372.DOI:10.16155/j.0254-1793.2006.10.024.
[29]曹亚飞,康健,常巧英,等.Qu ECh ERS结合液相色谱-串联质谱法快速测定奶酪种多种兽药残留[J].色谱,2015,33(2):132-139.DOI:10.3724/SP.J.1123.2014.10022.
[30]卜明楠,石志红,康健,等.Qu ECh ERS结合LC-MS/MS同时测定虾肉中72种兽药残留[J].分析测试学报,2012,31(5):552-558.DOI:10.3969/j.issn.1004-4957.2012.05008.
[2]李巧玲,刘景艳.市场鲜猪肉掺假状况的调查监测[J].食品科学,2004,25(10):273-276.
[3]程灵豪,王余良,林绍伟.PSE肉、注水肉、注胶肉的主要危害及检验方法[J].浙江畜牧兽医,2015(3):13-15.DOI:10.3969/j.issn.1005-7307.2015.03.005.
[4]王飒爽,陈永超,李文辉.注水肉的危害及检验方法分析[J].现代农业科技,2007(16):178-179.
[5]林荣泉.畜禽注水肉的特征与卫生检验[J].肉类研究,2001,15(3):38-51.
[6]BERTRAMH C,SCHAFER A,ROSENVOLD K,et al.Physical changes of significance for early mortem water distribution in porcine M.longissimus[J].Meat Science,2004,66(4):915-924.DOI:10.1016/S0309-1740(03)00188-8.
[7]仇国琴,郭乃勇,张艳.注水肉的危害与控制措施[J].中国畜牧兽医文摘,2014,30(12):22;76.
[8]黄琴,孙宏文,陈志刚.“注水肉”泛滥的原因及控制措施[J].中国畜牧兽医文摘,2012,28(2):186;148.
[9]吴兆良.猪肉水分限量标准与注水肉判断的研讨[J].肉类工业,2013(2):41-42.
[10]蒋腾.如何辨别注水肉[J].中国防伪报道,2016(10):111-113.
[11]黄玉萍,陈桂云,夏建春,等.注水肉无损检测技术现状与发展趋势分析[J].农业机械学报,2015,46(1):207-215.DOI:10.6041/j.issn.1000-1298.2015.01.030.
[12]郝冬梅,周亚男,王玉,等.基于可见-近红外光谱与稀疏表示的注水肉识别[J].光谱学与光谱分析,2015,35(1):93-98.DOI:10.3964/j.is sn.1000-0593(2015)01-0093-06.
[13]MAJA P,MARJETA C P,DAJAN S.Predicting pork water-holding capacity with NIR spectroscopy in relation to different reference methods[J].Journal of Food Engineering,2010,98(3):347-352.DOI:10.1016/j.jfoodeng.2009.11.022.
[14]王欣,王志永,陈利华,等.注水肉糜的低场核磁驰豫特性及判别分析[J].现代食品科技,2016,32(5):79-84.DOI:10.13982/j.mfst.1673-9078.2016.5.013.
[15]GUDJONSDOTTIR M,ARASON S,RUSTAD T.The effects of pre-salting methods on water distribution and protein denaturation of dry salted and rehydrated cod-A low-field NMR study[J].Journal of Food Engineering,2011,104(1):23-29.DOI:10.1016/j.jfoodeng.2010.11.022.
[16]郭培源,王昕琨,林岩,等.基于多传感器信息融合的注水肉检测方法研究[J].激光与光电子学进展,2013(7):1-7.DOI:10.3788/LOP50.073002.
[17]胡兴娟,吴宁鹏,孟蕾,等.超高效液相色谱-串联质谱法测定猪肉、猪肝及猪尿中的阿托品残留[J].中国兽药杂志,2014,48(7):46-49.
[18]刘谷欲,潘颖,陈桂良.猪血浆中阿托品含量的毛细管气相色谱测定[J].中国医药工业杂志,2003,34(5):241-242.
[19]毛谊平,任荣军,吴高芬.苍术中非法添加硫酸阿托品及氢溴酸东莨菪碱的检测方法[J].中国药业,2010,19(14):47-49.DOI:10.3969/j.issn.1006-4931.2010.14.031.
[20]韦寿莲,莫金垣,郑一宁.一种简单快速的高效毛细管电泳分离检测山莨菪碱和多沙唑嗪的方法[J].分析化学,2003,31(2):225-228.
[21]AZIZI S N,CHAICHI M J,SHAKERI P,et al.Determination of atropine using Mn-doped Zn S quantum dots as novel luminescent sensitizers[J].Journal of Luminescence,2013,144(12):34-40.DOI:10.1016/j.jlumin.2013.05.054.
[22]CHEN H P,SAEZ J M,GONZALEZ R R,et al.Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified Qu ECh ERs and liquid chromatography tandam mass spectrometry[J].Food Chemistry,2017,218:173-180.DOI:10.1016/j.foodchem.2016.09.075.
[23]SRAMSKA P,MACIEJKA A,TOPOLEWSKA A,et al.Isolation of atropine and scopolamine from plant material using liquid-liquid extraction and extrelut columns[J].Journal of Chromatography B,2017,1043:202-208.DOI:10.1016/j.jchromb.2016.09.003.
[24]SAEZ J M,GONZALEZ R R,FRENICH A G,et al.Enantiomeric determination and evaluation of the racemization process of atropine in Solanaceae seeds and contaminated samples by high performance liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A,2016,1474:79-84.DOI:10.1016/j.chroma.2016.10.047.
[25]KOZELJ G,PERHARIC L,STANOVNIK L,et al.Simple validated LC-MS/MS method for the determination of atropine and scopolamine in plasma for clinical and forensic toxicological purposes[J].Journal of Pharmaceutical and Biomedical Analysis,2014,96:197-206.DOI:10.1016/j.jpba.2014.03.037.
[26]刘谷歌,潘颖,陈桂良.猪血浆中阿托品含量的毛细管气相色谱测定[J].中国医药工业杂志,2003,34(5):132-139.DOI:10.3969/j.issn.1001-8255.2003.05.014.
[27]胡兴娟,吴宁鹏,董瑞静,等.UPLC-MS/MS测定4种兽药制剂中非法添加阿托品的方法研究[J].中国兽药杂志,2014,48(7):49-52.
[28]陈怀侠,杜鹏,韩凤梅,等.液相色谱-串联质谱法鉴定大鼠血浆中的阿托品及其代谢物[J].药物分析杂志,2006,26(10):1369-1372.DOI:10.16155/j.0254-1793.2006.10.024.
[29]曹亚飞,康健,常巧英,等.Qu ECh ERS结合液相色谱-串联质谱法快速测定奶酪种多种兽药残留[J].色谱,2015,33(2):132-139.DOI:10.3724/SP.J.1123.2014.10022.
[30]卜明楠,石志红,康健,等.Qu ECh ERS结合LC-MS/MS同时测定虾肉中72种兽药残留[J].分析测试学报,2012,31(5):552-558.DOI:10.3969/j.issn.1004-4957.2012.05008.