液相色谱-串联质谱法检测中兽药中非法添加氟喹诺酮类药物含量的不确定度评估
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摘要
目的评估液相色谱-串联质谱法检测中兽药中非法添加氟喹诺酮类药物含量的不确定度。方法建立液相色谱-串联质谱法检测中兽药(肥猪散、健胃散、银翘散)中非法添加氟喹诺酮类药物的含量测定方法,根据JJF1059.1-2012《测量不确定度评定与表示》的相关规定,对该方法的不确定度进行评定。结果中兽药中氟喹诺酮类药物含量分别为C(Enro)=100.90 mg/kg、C(Cip)=100.34 mg/kg、C(Norf)=100.21 mg/kg、C(Oflo)=100.61 mg/kg时,95%置信水平下,取k=2,不确定度评估结果分别表示为X(Enro)=(100.90±6.957)mg/kg;X(Cip)=(100.34±7.067) mg/kg; X(Norf)=(100.21±6.898) mg/kg; X(Oflo)=(100.61±6.957) mg/kg。结论评定结果表明,影响检测结果的主要因素为液相色谱-串联质谱仪的灵敏度、天平的精密度、操作的规范性。
Objective To evaluate the uncertainty of determination of fluoroquinolones illegally added in veterinary medicine by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods A method for the determination of fluoroquinolones illegally added in veterinary herbal medicine(feizhu powder, Jianwei powder,Yinqiao powder) by liquid chromatography-tandem mass spectrometry was established. According to the relevant provisions of JJF1059.1-2012 Measurement uncertainty evaluation and representation, the uncertainty of the method was evaluated. Results The content of fluoroquinolones in veterinary medicine was C(Enro)=100.90 mg/kg,C(Cip)=100.34 mg/kg, C(Norf)=100.21 mg/kg, C(Oflo)=100.61 mg/kg, respectively, when 95% confidence level,k=2, and the evaluation results were X(Enro)=(100.90±6.957) mg/kg, X(Cip)=(100.34±7.067) mg/kg, X(Norf)=(100.21±6.898) mg/kg, X(Oflo)=(100.61±6.957) mg/kg, respectively. Conclusion The main sources of uncertainty are the sensitivity of the liquid chromatography-tandem mass spectrometer, the precision of the balance, and the standard of operation.
Objective To evaluate the uncertainty of determination of fluoroquinolones illegally added in veterinary medicine by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods A method for the determination of fluoroquinolones illegally added in veterinary herbal medicine(feizhu powder, Jianwei powder,Yinqiao powder) by liquid chromatography-tandem mass spectrometry was established. According to the relevant provisions of JJF1059.1-2012 Measurement uncertainty evaluation and representation, the uncertainty of the method was evaluated. Results The content of fluoroquinolones in veterinary medicine was C(Enro)=100.90 mg/kg,C(Cip)=100.34 mg/kg, C(Norf)=100.21 mg/kg, C(Oflo)=100.61 mg/kg, respectively, when 95% confidence level,k=2, and the evaluation results were X(Enro)=(100.90±6.957) mg/kg, X(Cip)=(100.34±7.067) mg/kg, X(Norf)=(100.21±6.898) mg/kg, X(Oflo)=(100.61±6.957) mg/kg, respectively. Conclusion The main sources of uncertainty are the sensitivity of the liquid chromatography-tandem mass spectrometer, the precision of the balance, and the standard of operation.
引文
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[3]Seidel J,Clarke T,Mathew B.To cipro or not to ciprobilateral achilles ruptures with the use of quinolones[J].J Am Podiat Med Associat,2015,105(2):185-188.
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[8]倪海平,朱宝立,朱鸿儒.超高效液相色谱-串联质谱法测定鸡蛋中15种药物残留[J].食品安全质量检测学报,2018,8(9):3549-3555.Ni HP,Zhu BL,Zhu HR.Simultaneous determination of 15 drugs residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,8(9):3549-3555.
[9]肖英平,李玲,曾庆坤,等.高效液相色谱-三重四级杆质谱联用法检测荷斯坦和水牛原料乳中喹诺酮残留[J].食品安全质量检测学报,2016,7(9):3726-3731.Xiao YP,Li L,Zeng QK,et al.Determination of quinolone residues in raw Holstein and Buffalo milk by high performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2016,7(9):3726-3731.
[10]中华人民共和国农业部.农业部第2448号公告.附件2:第5条,肥猪散、健胃散、银翘散等中药散剂中非法添加氟喹诺酮类药物(物质)检查方法[EB/OL].[2016-09-22].http://www.moa.gov.cn/govpublic/SYJ/201609/t20160922_5282118.htm Ministry of Agriculture of the Peoples Republic of China.Ministry of Agriculture Announcement No 2448.Annex 2:Article 5,Examination method of illegally adding fluoroquinolones in traditional Chinese medicine powder such as Feizhu san,Jianwei san and Yinqiao san[EB/OL].[2016-09-22].http://www.moa.gov.cn/govpublic/SYJ/201609/t20160922_5282118.htm
[11]曹莹,蒋音.利用液质联用仪快速确证中兽药中的氟喹诺酮类药物[J].中国兽药杂志,2012,46(6):27-29.Cao Y,Jiang Y.Rapid confirmation of fluoroquinolones in traditional Chinese medicine by LC-MS[J].Chin J Vet Drug,2012,46(6):27-29.
[12]韩合敬,魏秀丽,邡智悲,等.超高效液相色谱-串联质谱法测定中兽药散剂中4种喹诺酮药物[J].黑龙江畜牧兽医,2017,(1):282-283,285Han H,Wei X,Hao ZH,et al.Determination of four quinolone drugs in veterinary traditional Chinese medicine powders by UPLC-MS[J].Heilongjiang Anim Sci Vet Med,2017,(1):282-283,285.
[13]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].
[14]CNAS-GL 06化学分析中不确定度的评估指南[S].CNAS-GL 06 Guidance on evaluation the uncertainty in chemical analysis[S].
[15]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification regulation of working glass container[S].
[16]JJF 646-2006移液器检定规程[S].JJF 646-2006 Verification regulation of locomotive pipette[S].
[2]张冬冬,苏超,洪伟,等.动物源食品中氟喹诺类兽药残留检测的研究进展[J].安徽农学通报,2016,22(13):38-41.Zhang DD,Su C,Hong W,et al.Advances in the detection of fluoroquinolones residues in animal-derived foods[J].Anhui Agric Sci Bull,2016,22(13):38-41.
[3]Seidel J,Clarke T,Mathew B.To cipro or not to ciprobilateral achilles ruptures with the use of quinolones[J].J Am Podiat Med Associat,2015,105(2):185-188.
[4]李华强,李素琴,丁真真.氟喹诺酮类抗菌药物的交叉耐药性分析[J].公共卫生与临床医学,2009,(4):271-274.Li HQ,Li SQ,Ding ZZ.Cross-resistance analysis of fluoroquinolones[J].Publ Health Clin Med,2009,(4):271-274.
[5]Niwa H,Chuma T,Okamoto K,et al.Simultaneous detection of mutations associated with resistance to macrolides and quinolones in Campylobacter jejuni and C.coli using a PCR-line probe assay[J].Int J Antimicrob Agents,2003,22(4):374-379.
[6]中华人民共和国农业部.农业部第2292号公告[EB/OL].[2015-9-7].http://www.moa.gov.cn/govpublic/SYJ/201509/t20150907_4819267.htm.Ministry of Agriculture of the Peoples Republic of China.Ministry of Agriculture Announcement No 2292[EB/OL].[2015-9-7].http://www.moa.gov.cn/govpublic/SYJ/201509/t20150907_4819267.htm.
[7]范维,高晓月,陈超,等.动物源性食品中喹诺酮类药物残留的检测[J].肉类研究,2017,31(4):36-42.Fan W,Gao XY,Chen C,et al.Screening and confirmation of quinolones residues in animal-derived food[J].Meat Res,2017,31(4):36-42.
[8]倪海平,朱宝立,朱鸿儒.超高效液相色谱-串联质谱法测定鸡蛋中15种药物残留[J].食品安全质量检测学报,2018,8(9):3549-3555.Ni HP,Zhu BL,Zhu HR.Simultaneous determination of 15 drugs residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,8(9):3549-3555.
[9]肖英平,李玲,曾庆坤,等.高效液相色谱-三重四级杆质谱联用法检测荷斯坦和水牛原料乳中喹诺酮残留[J].食品安全质量检测学报,2016,7(9):3726-3731.Xiao YP,Li L,Zeng QK,et al.Determination of quinolone residues in raw Holstein and Buffalo milk by high performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2016,7(9):3726-3731.
[10]中华人民共和国农业部.农业部第2448号公告.附件2:第5条,肥猪散、健胃散、银翘散等中药散剂中非法添加氟喹诺酮类药物(物质)检查方法[EB/OL].[2016-09-22].http://www.moa.gov.cn/govpublic/SYJ/201609/t20160922_5282118.htm Ministry of Agriculture of the Peoples Republic of China.Ministry of Agriculture Announcement No 2448.Annex 2:Article 5,Examination method of illegally adding fluoroquinolones in traditional Chinese medicine powder such as Feizhu san,Jianwei san and Yinqiao san[EB/OL].[2016-09-22].http://www.moa.gov.cn/govpublic/SYJ/201609/t20160922_5282118.htm
[11]曹莹,蒋音.利用液质联用仪快速确证中兽药中的氟喹诺酮类药物[J].中国兽药杂志,2012,46(6):27-29.Cao Y,Jiang Y.Rapid confirmation of fluoroquinolones in traditional Chinese medicine by LC-MS[J].Chin J Vet Drug,2012,46(6):27-29.
[12]韩合敬,魏秀丽,邡智悲,等.超高效液相色谱-串联质谱法测定中兽药散剂中4种喹诺酮药物[J].黑龙江畜牧兽医,2017,(1):282-283,285Han H,Wei X,Hao ZH,et al.Determination of four quinolone drugs in veterinary traditional Chinese medicine powders by UPLC-MS[J].Heilongjiang Anim Sci Vet Med,2017,(1):282-283,285.
[13]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].
[14]CNAS-GL 06化学分析中不确定度的评估指南[S].CNAS-GL 06 Guidance on evaluation the uncertainty in chemical analysis[S].
[15]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification regulation of working glass container[S].
[16]JJF 646-2006移液器检定规程[S].JJF 646-2006 Verification regulation of locomotive pipette[S].