分散固相萃取-高效液相色谱串联质谱法测定水产品中氯霉素类药物的残留量
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摘要
本文采用分散固相萃取技术作为前处理手段,结合高效液相色谱串联质谱(HPLC-MS/MS)高灵敏度和高选择性的优势,建立了一种水产品中氯霉素类药物残留的检测方法。实验探讨和优化了以分散固相萃取净化样液过程中的提取条件、固体吸附剂的用量等。并优化检测方法的色谱、质谱条件,采用多反应监测模式(MRM)对目标物进行定性、定量分析。结果表明,目标物在一定的浓度范围内具有良好的线性关系;方法的检出限为0.07～0.10μg·kg~(-1)。对样品进行三个水平加标实验,目标化合物的回收率为88.81%～102.89%,相对标准偏差(RSD,n=6)为2.30%～4.87%。该方法定性定量准确,灵敏度高,有效去除基质干扰,适用于水产品中氯霉素类药物残留量的定性、定量分析。
A new approach was established for the determination of choramphenicols residues in aquatic products,base on the combination of dispersive solid-phase extraction(DSPE)method and high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)technology. The extraction conditions and the amount of solid adsorbent used by DSPE during the sample purification were studied and optimized. The chromatographic and mass spectrometric conditions were op?timized too,and the targets was qualitatively and quantitatively analyzed by multi-reaction monitoring mode(MRM). Re?sults showed that all analytes responding to signal had a fine linear relationship,and their detection limits ranged from 0.07～0.10 μg·kg~(-1). Three horizontal recovery experiments were carried out,the average recoveries were 88.81%～102.89% and the RSD were 2.30%～4.87%. This method has the advantages of accurate analysis,high sensitivity,effective removal of matrix interference,and is suitable for the qualitative and quantitative analysis of chloramphenicols in aquatic products.
A new approach was established for the determination of choramphenicols residues in aquatic products,base on the combination of dispersive solid-phase extraction(DSPE)method and high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)technology. The extraction conditions and the amount of solid adsorbent used by DSPE during the sample purification were studied and optimized. The chromatographic and mass spectrometric conditions were op?timized too,and the targets was qualitatively and quantitatively analyzed by multi-reaction monitoring mode(MRM). Re?sults showed that all analytes responding to signal had a fine linear relationship,and their detection limits ranged from 0.07～0.10 μg·kg~(-1). Three horizontal recovery experiments were carried out,the average recoveries were 88.81%～102.89% and the RSD were 2.30%～4.87%. This method has the advantages of accurate analysis,high sensitivity,effective removal of matrix interference,and is suitable for the qualitative and quantitative analysis of chloramphenicols in aquatic products.
引文
[1]杨洪波,王荻,卢彤岩.氯霉素类药物的药理学在水产动物中的研究现状[J].水产学杂志,2013,26(4):61-64.
[2]孙伟红,刘欢,邢丽红,等.水产品兽药残留检测技术标准解析及能力验证工作探讨[J].中国渔业质量与标准,2017,7(2):11-18.
[3]胡顶飞,沈建忠.氯霉素类抗生素的残留分析[J].中国兽药杂志,2001,35(5):55-57.
[4]朱文嘉,王联珠,郭莹莹,等.国内外鱼类产品兽药残留限量标准对比分析[J].水产科技情报,2013,40(5):225-231.
[5]王安伟,刘天密,覃锐,等.水产品中氯霉素残留检测方法研究进展[J].食品安全质量检测学报,8(11):4259-4264.
[6]赵霞,王波,谢恺舟,等.动物性食品中氯霉素类药物残留色谱和质谱检测技术研究进展[J].分析试验室,2018,37(8):978-985.
[7]中华人民共和国农业部.农业部958号公告-14-2007水产品中氯霉素、甲砜霉素、氟甲砜霉素残留量的测定气相色谱-质谱法[S].北京:中国标准出版社,2007.
[8]熊春兰,郭平,占春瑞,等.高效液相色谱-串联质谱法同时测定水产品中8类38种兽药残留[J].分析测试学报,2013,32(2):193-198.
[9]陈京都,吴红军,成强,等.液相色谱-质谱联用技术在水产品兽药残留检测中的应用[J].化学分析计量,2015,24(5):105-107.
[10]王淼,王艳,吴艳云,等. QuEChERS方法在水产品药物残留检测中的应用研究进展[J].现代农业科技,2017,9(17):257-259.
[11]陈国栋,王颖.检测水产品中兽药残留的QuEChERS方法应用研究[J].食品安全导刊,2015,8(33):159-161.
[12]卜明楠,石志红,康健,等. QuEChERS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.
[13]高何刚.氯霉素残留的液相色谱质谱检测方法的样品前处理研究进展[J].广州化工,2017,44(8):204-205.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 22338-2008动物源性食品中氯霉素类药物残留量测定[S].北京:中国标准出版社,2008.
[2]孙伟红,刘欢,邢丽红,等.水产品兽药残留检测技术标准解析及能力验证工作探讨[J].中国渔业质量与标准,2017,7(2):11-18.
[3]胡顶飞,沈建忠.氯霉素类抗生素的残留分析[J].中国兽药杂志,2001,35(5):55-57.
[4]朱文嘉,王联珠,郭莹莹,等.国内外鱼类产品兽药残留限量标准对比分析[J].水产科技情报,2013,40(5):225-231.
[5]王安伟,刘天密,覃锐,等.水产品中氯霉素残留检测方法研究进展[J].食品安全质量检测学报,8(11):4259-4264.
[6]赵霞,王波,谢恺舟,等.动物性食品中氯霉素类药物残留色谱和质谱检测技术研究进展[J].分析试验室,2018,37(8):978-985.
[7]中华人民共和国农业部.农业部958号公告-14-2007水产品中氯霉素、甲砜霉素、氟甲砜霉素残留量的测定气相色谱-质谱法[S].北京:中国标准出版社,2007.
[8]熊春兰,郭平,占春瑞,等.高效液相色谱-串联质谱法同时测定水产品中8类38种兽药残留[J].分析测试学报,2013,32(2):193-198.
[9]陈京都,吴红军,成强,等.液相色谱-质谱联用技术在水产品兽药残留检测中的应用[J].化学分析计量,2015,24(5):105-107.
[10]王淼,王艳,吴艳云,等. QuEChERS方法在水产品药物残留检测中的应用研究进展[J].现代农业科技,2017,9(17):257-259.
[11]陈国栋,王颖.检测水产品中兽药残留的QuEChERS方法应用研究[J].食品安全导刊,2015,8(33):159-161.
[12]卜明楠,石志红,康健,等. QuEChERS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.
[13]高何刚.氯霉素残留的液相色谱质谱检测方法的样品前处理研究进展[J].广州化工,2017,44(8):204-205.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 22338-2008动物源性食品中氯霉素类药物残留量测定[S].北京:中国标准出版社,2008.