液相色谱串联质谱法测定肉糜中克伦特罗残留量的不确定度评定
|
摘要
目的评定液相色谱-质谱/质谱法测定肉糜中克伦特罗残留量的不确定度。方法根据JJF1059.1-2012《测量不确定度评定与表示》,考察称量、标准溶液的配制、样品提取净化、仪器测量等主要因素引入的不确定度,并对不确定度的各分量进行计算和合成。结果该方法测定肉糜中克伦特罗残留量的合成相对标准不确定度为0.0428,肉糜中克伦特罗残留量测定结果为(18.8±1.6)μg/kg(P=95%,k=2)。结论本实验的不确定度主要由标准溶液与内标物的峰面积比、样品与内标物的峰面积比、标准溶液和样品中内标物的浓度比引入。
Objective To evaluate the uncertainty of determination of clenbuterol in meat by liquid chromatography tandem mass spectrometry. Methods According to JJF 1059.1-2012 Measurement uncertainty evaluation and presentation, the uncertainty of main factors such as weighing, standard solution preparation, sample extraction and purification, apparatus measure were investigated, and the components of uncertainty were calculated and synthesized. Results The synthetic relative standard uncertainty of the method for the determination of clenbuterol residues in meat emulsion was 0.0428. The determination results of clenbuterol residues in mince meat was(18.8±1.6) μg/kg(P=95%, k=2). Conclusion The uncertainty of the method is mainly caused by peak area ratio of standard solution and internal standard, peak area ratio of sample and internal standard and concentration ratio of internal standard in standard solution and sample.
Objective To evaluate the uncertainty of determination of clenbuterol in meat by liquid chromatography tandem mass spectrometry. Methods According to JJF 1059.1-2012 Measurement uncertainty evaluation and presentation, the uncertainty of main factors such as weighing, standard solution preparation, sample extraction and purification, apparatus measure were investigated, and the components of uncertainty were calculated and synthesized. Results The synthetic relative standard uncertainty of the method for the determination of clenbuterol residues in meat emulsion was 0.0428. The determination results of clenbuterol residues in mince meat was(18.8±1.6) μg/kg(P=95%, k=2). Conclusion The uncertainty of the method is mainly caused by peak area ratio of standard solution and internal standard, peak area ratio of sample and internal standard and concentration ratio of internal standard in standard solution and sample.
引文
[1]JJF 1135-2005化学分析测量不确定度评定[S].JJF 1135-2005 Evaluation of uncertainty in chemical analysis measurement[S].
[2]CNAS-CL 01-A002检测和校准实验室能力认可准则在化学检测领域的应用说明[S].CNAS-CL 01-A002 Guidance on the application of testing and calibration laboratories competence accreditation criteria in the field of chemical testing[S].
[3]高亦军,罗冠中.肉制品中瘦肉精药物残留检测方法的简化研究[J].食品研究与开发,2012,33(8):141-144.Gao YJ,Luo GZ.Research on simplified detection method of clenbuterol residues in meat product[J].Food Res Dev,2012,33(8):141-144.
[4]罗宿星,黄丽娟,伍远辉.肉制品中瘦肉精的检测方法[J].遵义师范学院学报,2014,16(6):74-77.Luo SX,Huang LJ,Wu YH.Detection method of clenbuterol in meta products[J].J Zunyi Norm Coll,2014,16(6):74-77.
[5]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[S].
[6]CNAS-GL 06化学分析中不确定度的评估指南[S].CNAS-GL 06 Guidance on evaluating the uncertainty in chemical analysis[S].
[7]SN/T 1924-2011进出口动物源食品中克伦特罗、莱克多巴胺、沙丁胺醇和特布他林残留量的测定液相色谱-质谱/质谱法[S].SN/T 1924-2011 Determination of clenbuterol,ractopamine,salbutemol and terbutalin residue in foodstuffs of animal origin for import and export-Liquid chromatography-mass spectrometry/mass spectrometry[S].
[8]JJF 196-2006常用玻璃量器检定规程[S].JJF 196-2006 Verification regulation of working glass container[S].
[9]JJF 646-2006移液器检定规程[S].JJF 646-2006 Verification regulation of locomotive pipette[S].
[10]秦立,肖英,王莹,等.HPLC法测定泼尼松龙原料药含量的测量不确定度评定[J].中国药房,2015,26(13):4737-4739.Qin L,Xiao Y,Wang Y,et al.Uncertainty measurement evaluation of the content determination of prednisolone API by HPLC[J].China Pharm,2015,26(13):4737-4739.
[11]董玲玲,于晓辉,杨星,等.气相色谱内标法测定双甲脒溶液含量的不确定评定[J].中国兽药杂志,2017,51(5):33-36.Dong LL,Yu XH,Yang X,et al.Evaluation of uncertainty of determination of amitraz solution by the GC internal standard method[J].Chin J Veter Drug,2017,51(5):33-36.
[12]董晓杰,董兵,刘峰平,等.气相色谱内标法测定消毒剂中乙醇含量的不确定度评定[J].中国消费学杂志,2017,34(12):1096-1099.Dong XJ,Dong B,Liu FP,et al.Evaluation of uncertainty of ethanol content in disinfectant by gas chromatography with internal standard curve method[J].Chin J Disinfectant,2017,34(12):1096-1099.
[13]宁霄,金绍明,梁瑞强,等.超高效液相色谱-串联质谱法测定猪肉中β-受体激动剂残留量的不确定度分析[J].食品科学,2017,38(6):315-320.Ning X,Jin SM,Liang RQ,et al.Uncertainty evaluation for the determination ofβ-agonists in pork by ultra performance liquid chromatography-tandem mass spectrometry[J].Food Sci,2017,38(6):315-320.
[14]官咏仪,邱志超,宋阳,等.高效液相色谱法测定葡萄酒中山梨酸含量的不确定度评定[J].食品科学,2015,36(16):231-235.Guan YY,Qiu ZC,Song Y,et al.Uncertainty evaluation for determining sorbic acid in wine by high performance liquid chromatography[J].Food Sci,2015,36(16):231-235.
[15]倪永付,王勇,朱莉萍,等.液相色谱-串联质谱法测定肠衣中克伦特罗残留量不确定度分析[J].肉类工业,2012,374(6):46-49.Ni YF,Wang Y,Zhu LP,et al.Analysis on uncertainty in measuring clenbuterol in casing by LC-MS/MS[J].Meat Ind,2012,374(6):46-49.
[2]CNAS-CL 01-A002检测和校准实验室能力认可准则在化学检测领域的应用说明[S].CNAS-CL 01-A002 Guidance on the application of testing and calibration laboratories competence accreditation criteria in the field of chemical testing[S].
[3]高亦军,罗冠中.肉制品中瘦肉精药物残留检测方法的简化研究[J].食品研究与开发,2012,33(8):141-144.Gao YJ,Luo GZ.Research on simplified detection method of clenbuterol residues in meat product[J].Food Res Dev,2012,33(8):141-144.
[4]罗宿星,黄丽娟,伍远辉.肉制品中瘦肉精的检测方法[J].遵义师范学院学报,2014,16(6):74-77.Luo SX,Huang LJ,Wu YH.Detection method of clenbuterol in meta products[J].J Zunyi Norm Coll,2014,16(6):74-77.
[5]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[S].
[6]CNAS-GL 06化学分析中不确定度的评估指南[S].CNAS-GL 06 Guidance on evaluating the uncertainty in chemical analysis[S].
[7]SN/T 1924-2011进出口动物源食品中克伦特罗、莱克多巴胺、沙丁胺醇和特布他林残留量的测定液相色谱-质谱/质谱法[S].SN/T 1924-2011 Determination of clenbuterol,ractopamine,salbutemol and terbutalin residue in foodstuffs of animal origin for import and export-Liquid chromatography-mass spectrometry/mass spectrometry[S].
[8]JJF 196-2006常用玻璃量器检定规程[S].JJF 196-2006 Verification regulation of working glass container[S].
[9]JJF 646-2006移液器检定规程[S].JJF 646-2006 Verification regulation of locomotive pipette[S].
[10]秦立,肖英,王莹,等.HPLC法测定泼尼松龙原料药含量的测量不确定度评定[J].中国药房,2015,26(13):4737-4739.Qin L,Xiao Y,Wang Y,et al.Uncertainty measurement evaluation of the content determination of prednisolone API by HPLC[J].China Pharm,2015,26(13):4737-4739.
[11]董玲玲,于晓辉,杨星,等.气相色谱内标法测定双甲脒溶液含量的不确定评定[J].中国兽药杂志,2017,51(5):33-36.Dong LL,Yu XH,Yang X,et al.Evaluation of uncertainty of determination of amitraz solution by the GC internal standard method[J].Chin J Veter Drug,2017,51(5):33-36.
[12]董晓杰,董兵,刘峰平,等.气相色谱内标法测定消毒剂中乙醇含量的不确定度评定[J].中国消费学杂志,2017,34(12):1096-1099.Dong XJ,Dong B,Liu FP,et al.Evaluation of uncertainty of ethanol content in disinfectant by gas chromatography with internal standard curve method[J].Chin J Disinfectant,2017,34(12):1096-1099.
[13]宁霄,金绍明,梁瑞强,等.超高效液相色谱-串联质谱法测定猪肉中β-受体激动剂残留量的不确定度分析[J].食品科学,2017,38(6):315-320.Ning X,Jin SM,Liang RQ,et al.Uncertainty evaluation for the determination ofβ-agonists in pork by ultra performance liquid chromatography-tandem mass spectrometry[J].Food Sci,2017,38(6):315-320.
[14]官咏仪,邱志超,宋阳,等.高效液相色谱法测定葡萄酒中山梨酸含量的不确定度评定[J].食品科学,2015,36(16):231-235.Guan YY,Qiu ZC,Song Y,et al.Uncertainty evaluation for determining sorbic acid in wine by high performance liquid chromatography[J].Food Sci,2015,36(16):231-235.
[15]倪永付,王勇,朱莉萍,等.液相色谱-串联质谱法测定肠衣中克伦特罗残留量不确定度分析[J].肉类工业,2012,374(6):46-49.Ni YF,Wang Y,Zhu LP,et al.Analysis on uncertainty in measuring clenbuterol in casing by LC-MS/MS[J].Meat Ind,2012,374(6):46-49.
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |