猪肉中磺胺类兽药残留基体标准物质高准确度定值方法
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摘要
建立了猪肉中磺胺类兽药残留基体标准物质高准确度定值方法,优化了提取溶剂、提取次数、添加内标试剂后的平衡时间和过滤膜的选择等样品前处理条件。猪肉样品中加入同位素标记物,乙腈提取3次,上清液过无水硫酸钠柱,提取物经50℃水浴旋转蒸发至干,正己烷饱和的流动相定容溶解,正己烷脱脂净化,然后正离子多反应监测测定,最后采用外标法定量。结果表明,磺胺嘧啶和磺胺二甲嘧啶在10. 0～200. 0 ng/m L浓度范围内呈良好的线性关系,线性相关系数均大于0. 999,方法的检出限和定量限分别为0. 5、2. 0μg/kg,在低、中、高3个添加水平范围内的回收率为95. 7%～104. 8%,相对标准偏差<5%(n=6),可用于猪肉中磺胺类兽药残留基体标准物质均匀性检验、稳定性监测和定值。
A highly accurate quantification method was established for the determination of sulfonamides residues in pork for a matrix reference material. Several key issues during the sample pretreatment were optimized including extraction solvent,times of sample extraction,equilibration time after the addition of internal standards,the selection of filter membrane. Internal standards were added into the sample,and then the sample was extracted 3 times by acetonitrile and centrifugation.The supernatant was then treated with a home-made separation column filled with anhydrous sodium sulfate.The extract was evaporated and dried by rotary evaporator at the temperature of 50 ℃.The residue was dissolved by mobile phase saturated with n-hexane,and it was defatted and purified by n-hexane.The analysis was performed under the positive mode using multiple reaction monitoring(MRM) and quantified by external standard method.A good linearity was obtained in the range from 10. 0 to 200. 0 ng/m L for sulfadiazine and sulfadimidine,while the correlation coefficients were more than 0. 999.The limits of detection(LODs) and the limits of quantitation(LOQs) were 0. 5 μg/kg and 2. 0 μg/kg respectively. The recovery rates at the three spiked levels were between 95. 7% ～104. 8% with relative standard deviations(RSDs,n = 6) less than 5%.The method was suitable for the homogeneity inspection,stability monitoring and certify value of the matrix reference materials for sulfonamides residues in pork.
A highly accurate quantification method was established for the determination of sulfonamides residues in pork for a matrix reference material. Several key issues during the sample pretreatment were optimized including extraction solvent,times of sample extraction,equilibration time after the addition of internal standards,the selection of filter membrane. Internal standards were added into the sample,and then the sample was extracted 3 times by acetonitrile and centrifugation.The supernatant was then treated with a home-made separation column filled with anhydrous sodium sulfate.The extract was evaporated and dried by rotary evaporator at the temperature of 50 ℃.The residue was dissolved by mobile phase saturated with n-hexane,and it was defatted and purified by n-hexane.The analysis was performed under the positive mode using multiple reaction monitoring(MRM) and quantified by external standard method.A good linearity was obtained in the range from 10. 0 to 200. 0 ng/m L for sulfadiazine and sulfadimidine,while the correlation coefficients were more than 0. 999.The limits of detection(LODs) and the limits of quantitation(LOQs) were 0. 5 μg/kg and 2. 0 μg/kg respectively. The recovery rates at the three spiked levels were between 95. 7% ～104. 8% with relative standard deviations(RSDs,n = 6) less than 5%.The method was suitable for the homogeneity inspection,stability monitoring and certify value of the matrix reference materials for sulfonamides residues in pork.
引文
[1]段振娟,张鸿雁,王硕.动物性食品中磺胺类药物残留分析研究进展[J].食品研究与开发,2007,28(6):149-152.
[2]任丹丹,谢云峰,李少晖,等.超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留[J].食品安全质量检测学报,2018,9(4):858-863.
[3]靳红果,张瑞,王颖,等.我国猪肉中磺胺类药物的残留特征分析[J].肉类研究,2017,31(10):31-35.
[4]徐慧敏,蔡宏文,李天元,等.磺胺类药物过敏和交叉过敏的研究进展[J].中国药理学与毒理学杂志,2012,26(6):897-902.
[5]BARAN W,ADAMEK E,ZIEMIANSKA J,et al.Effect ofthe presence of sulfonamides in the environment and theirinfluence on human health[J]. J. Hazard. Mater.,2011,196(30):1-15.
[6]金磊,姜蕾,韩琪,等.华东地区某水源水中13种磺胺类抗生素的分布特征及人体健康风险评价[J].环境科学,2016,37(7):2 515-2 521.
[7]吴敏,陈相宇.高效液相色谱法测定猪肉中五种磺胺类药物残留量[J].中国畜牧兽医文摘,2017,33(1):72.
[8]尹太坤,杨方,刘正才,等.鳗鲡肌肉中喹诺酮类及磺胺类药物残留基体标准物质的研制[J].中国测试,2016,40(4):54-59.
[9]张元,李伟青,周伟娥,等.食品中磺胺类药物前处理及检测方法研究进展[J].食品科学,2015,36(23):340-346.
[10]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.畜禽肉中十六种磺胺类药物残留量的测定液相色谱-串联质谱法:GB/T20759—2006[S].北京:中国标准出版社,2006.
[11]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.动物源性食品中磺胺类药物的残留量的测定液相色谱-质谱/质谱法:GB/T21316—2007[S].北京:中国标准出版社,2007.
[12]杨梅,孙思,王安波,等.超高效液相色谱-串联质谱法测定猪肉中磺胺类药物残留量[J].食品安全质量检测学报,2017,8(9):3633-3638.
[13]吴淑秀,公茂金,朱万燕,等.液相色谱串联质谱法测定猪肉和猪肝中9种磺胺类药物的残留[J].分析实验室,2012,31(2):79-83.
[14]吴云丽.液相微萃取技术及其在高效液相色谱分析中的应用[D].武汉:武汉大学,2010.
[15]中华人民共和国国家质量监督检验检疫总局.出口猪肉、虾、蜂蜜中多类药物残留量的测定液相色谱-质谱/质谱法:SN/T 3155—2012[S].北京:中国标准出版社,2012.
[16]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.河豚鱼、鳗鱼中十八种磺胺类药物残留量的测定液相色谱-串联质谱法:GB/T22951—2008[S].北京:中国标准出版社,2008.
[17]庞国芳,曹彦忠,张进杰,等.液相色谱-串联质谱同时测定家禽组织中16种磺胺残留[J].分析化学,2005,33(9):1 252-1 256.
[18]农业部1025号公告-23—2008.动物源食品中磺胺类药物残留检测液相色谱-串联质谱法[S].北京:中国标准出版社,2008.
[19]孙雷,毕言锋,李丹,等.猪肉中磺胺类药物残留检测能力验证分析[J].中国兽药杂志,2012,46(2):23-26.
[20]刘佳佳,佘永新,刘洪斌,等.高效液相色谱-串联质谱法同时测定动物源性食品中24种磺胺类药物残留[J].分析试验室,2011,30(2):9-13.
[21]TRUFELLI H,PALMA P,FAMIGLINI G,et al.An over-view of matrix effects in liquid chromatography-massspectrometry[J].Mass Spectrom.Rev.,2011,30(3):491-509.
[22]DE NARDI C,BONELLI F.Moving from fast to ballisticgradient in liquid chromatography/tandem mass spec-trometry pharmaceutical bioanalysis:matrix effect andchromatographic evaluations[J]. Rapid Commum. MassSpectrom.,2006,20(18):2 709-2 716.
[2]任丹丹,谢云峰,李少晖,等.超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留[J].食品安全质量检测学报,2018,9(4):858-863.
[3]靳红果,张瑞,王颖,等.我国猪肉中磺胺类药物的残留特征分析[J].肉类研究,2017,31(10):31-35.
[4]徐慧敏,蔡宏文,李天元,等.磺胺类药物过敏和交叉过敏的研究进展[J].中国药理学与毒理学杂志,2012,26(6):897-902.
[5]BARAN W,ADAMEK E,ZIEMIANSKA J,et al.Effect ofthe presence of sulfonamides in the environment and theirinfluence on human health[J]. J. Hazard. Mater.,2011,196(30):1-15.
[6]金磊,姜蕾,韩琪,等.华东地区某水源水中13种磺胺类抗生素的分布特征及人体健康风险评价[J].环境科学,2016,37(7):2 515-2 521.
[7]吴敏,陈相宇.高效液相色谱法测定猪肉中五种磺胺类药物残留量[J].中国畜牧兽医文摘,2017,33(1):72.
[8]尹太坤,杨方,刘正才,等.鳗鲡肌肉中喹诺酮类及磺胺类药物残留基体标准物质的研制[J].中国测试,2016,40(4):54-59.
[9]张元,李伟青,周伟娥,等.食品中磺胺类药物前处理及检测方法研究进展[J].食品科学,2015,36(23):340-346.
[10]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.畜禽肉中十六种磺胺类药物残留量的测定液相色谱-串联质谱法:GB/T20759—2006[S].北京:中国标准出版社,2006.
[11]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.动物源性食品中磺胺类药物的残留量的测定液相色谱-质谱/质谱法:GB/T21316—2007[S].北京:中国标准出版社,2007.
[12]杨梅,孙思,王安波,等.超高效液相色谱-串联质谱法测定猪肉中磺胺类药物残留量[J].食品安全质量检测学报,2017,8(9):3633-3638.
[13]吴淑秀,公茂金,朱万燕,等.液相色谱串联质谱法测定猪肉和猪肝中9种磺胺类药物的残留[J].分析实验室,2012,31(2):79-83.
[14]吴云丽.液相微萃取技术及其在高效液相色谱分析中的应用[D].武汉:武汉大学,2010.
[15]中华人民共和国国家质量监督检验检疫总局.出口猪肉、虾、蜂蜜中多类药物残留量的测定液相色谱-质谱/质谱法:SN/T 3155—2012[S].北京:中国标准出版社,2012.
[16]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.河豚鱼、鳗鱼中十八种磺胺类药物残留量的测定液相色谱-串联质谱法:GB/T22951—2008[S].北京:中国标准出版社,2008.
[17]庞国芳,曹彦忠,张进杰,等.液相色谱-串联质谱同时测定家禽组织中16种磺胺残留[J].分析化学,2005,33(9):1 252-1 256.
[18]农业部1025号公告-23—2008.动物源食品中磺胺类药物残留检测液相色谱-串联质谱法[S].北京:中国标准出版社,2008.
[19]孙雷,毕言锋,李丹,等.猪肉中磺胺类药物残留检测能力验证分析[J].中国兽药杂志,2012,46(2):23-26.
[20]刘佳佳,佘永新,刘洪斌,等.高效液相色谱-串联质谱法同时测定动物源性食品中24种磺胺类药物残留[J].分析试验室,2011,30(2):9-13.
[21]TRUFELLI H,PALMA P,FAMIGLINI G,et al.An over-view of matrix effects in liquid chromatography-massspectrometry[J].Mass Spectrom.Rev.,2011,30(3):491-509.
[22]DE NARDI C,BONELLI F.Moving from fast to ballisticgradient in liquid chromatography/tandem mass spec-trometry pharmaceutical bioanalysis:matrix effect andchromatographic evaluations[J]. Rapid Commum. MassSpectrom.,2006,20(18):2 709-2 716.