超高效液相色谱-串联质谱检测鹌鹑蛋中氯霉素类药物残留
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摘要
建立鹌鹑蛋中氯霉素类药物残留的超高效液相色谱-串联质谱检测方法。鹌鹑蛋样品采用了液-液萃取(LLE)和加速溶剂萃取(ASE)两种样品前处理技术,乙腈饱和的正己烷去脂,净化后用超高效液相色谱-串联质谱(UPLC-MS/MS)仪进行分析。CAP,TAP,FF和FFA的添加浓度分别在0. 08～25μg/kg,0. 8～150μg/kg,0. 27～250μg/kg,1. 2～250μg/kg范围内,线性关系良好,决定系数均大于0. 9993。CAP,TAP,FF和FFA添加水平为LOQ,0. 5,1. 0和2. 0 M RL/M RPL时,平均回收率在91. 7%～106. 2%范围内,相对标准偏差(RSD)均低于3. 4%。4种目标化合物的检测限(LOD)和定量限(LOQ)的范围分别为0. 03～0. 4μg/kg和0. 08～1. 2μg/kg。
A method for the determination of chloramphenicols residues in quail eggs was established using ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry( UPLCMS/MS). Quail egg samples were extracted using two sample preparation techniques,including liquid-liquid extraction( LLE) and accelerated solvent extraction( ASE). Fat was removed by acetonitrile saturated with n-hexane,purified before analysis on UPLC-MS/MS system. At the fortified levels of 0. 08 ～ 25 μg/kg for CAP,0. 8 ～ 150 μg/kg for TAP,0. 27 ～ 250 μg/kg for FF and1. 2 ～ 250 μg/kg for FFA,the linear relationship was good,and the coefficient of determination was above 0. 9993. When the added concentration of CAP, TAP, FF and FFA were the limit of quantification( LOQ),0. 5,1. 0 and 2. 0 MRL or MRPL,the average recoveries were 91. 7% ～106. 2%,and the relative standard deviations( RSDs) were lower than 3. 4%. The limit of detection( LOD) and limit of quantitation( LOQ) for the four target compounds were 0. 03 ～ 0. 4 μg/kg and0. 08 ～ 1. 2 μg/kg,respectively.
A method for the determination of chloramphenicols residues in quail eggs was established using ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry( UPLCMS/MS). Quail egg samples were extracted using two sample preparation techniques,including liquid-liquid extraction( LLE) and accelerated solvent extraction( ASE). Fat was removed by acetonitrile saturated with n-hexane,purified before analysis on UPLC-MS/MS system. At the fortified levels of 0. 08 ～ 25 μg/kg for CAP,0. 8 ～ 150 μg/kg for TAP,0. 27 ～ 250 μg/kg for FF and1. 2 ～ 250 μg/kg for FFA,the linear relationship was good,and the coefficient of determination was above 0. 9993. When the added concentration of CAP, TAP, FF and FFA were the limit of quantification( LOQ),0. 5,1. 0 and 2. 0 MRL or MRPL,the average recoveries were 91. 7% ～106. 2%,and the relative standard deviations( RSDs) were lower than 3. 4%. The limit of detection( LOD) and limit of quantitation( LOQ) for the four target compounds were 0. 03 ～ 0. 4 μg/kg and0. 08 ～ 1. 2 μg/kg,respectively.
引文
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[3] U. S. Food and Drug Administration. CFR-Code of Federal regulations title 21 part 556 tolerances for residue of new animal drugs in food,2014
[4] Ministry of Agriculture of the People's Republic of China. Maxium Residue Level of Veterinary Drugs in Food of Animal Origin. Notice No. 235(Appendix 4). Beijing:Ministry of Agriculture,2002中华人民共和国农业部.动物性食品中兽药最高残留限量[S]//公告第235号(附录4).北京:农业部,2002
[5] Orlando E A,Costa Roque A G,Losekann M E,Colnaghi Simionato A V. J. Chromatogr. B.,2016,1035:8
[6] Pan X D,Wu P G,Jiang W,Ma B J. Food. Control.,2015,52:34
[7] Chen Q,Song Z C,Zhang C W,Zhu L. Chin. J. Vet. Drug.,2015,49(8):28陈蔷,宋志超,张崇威,朱雷.中国兽药杂志,2015,49(8):28
[8] Xiao Z,Song R,Rao Z,Wei S,Jia Z,Suo D,Fan X. J. Chromatogr. A.,2015,1418(4):29
[9] Cai X X,Zhang X Y. Chin. J. Health. Lab. Technol.,2009,19(2):258蔡欣欣,张秀尧.中国卫生检验杂志,2009,19(2):258
[10] Sun L,Zhang L,Wang S H,Wang X. Chin. J. Vet. Drug.,2009,43(3):42孙雷,张骊,王树槐,汪霞.中国兽药杂志,2009,43(3):42
[11] Pan X D,Wu P G,Jiang W. Chin. J. Food. Hygi.,2014,26(6):572潘晓东,吴平谷,姜维.中国食品卫生杂志,2014,26(6):572
[12] Ren J,Zheng X P,Huang F F,Chen J C,Ma Y Q,Lou F. Food&Machinery.,2011,27(4):75任佳,郑小平,黄菲菲,陈景春,马颖清,楼飞.食品与机械,2011,27(4):75
[13] Jia H X,Zhou M,Lin S. Chin. J. Health. Lab. Technol.,2013,25(13):2726贾宏新,邹淼,林盛.中国卫生检验杂志,2013,25(13):2726
[14] Yang J,Yang Z,Yu Z,Li X R,Zhang J N,Zhang H Z. Chin. J. Anal. Lab.,2016,35(12):1463杨洁,杨钊,于宙,李新荣,张军宁,张辉珍.分析试验室,2016,35(12):1463
[15] Zeng Y,Dong W T,Gong B,Zhou Q,Jin L. Chin. J. Vet. Drug.,2017,51(12):42曾勇,董文婷,龚波,周青,金灵.中国兽药杂志,2017,51(12):42