LC-si正相固相萃取-HPLC-MS/MS法测定乌鸡白凤丸中氯霉素残留
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摘要
目的:建立正相固相萃取结合液质联用测定乌鸡白凤丸(水蜜丸)中氯霉素残留量方法。方法:采用LC-si硅胶正相固相萃取柱净化富集样品,高效液相-电喷雾-串联四极杆质谱法测定乌鸡白凤丸中氯霉素的残留量,使用Agilent-ODS C18(250mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水梯度洗脱,(0~7 min,30%甲醇;7~15 min,30%~80%甲醇;15~25 min,80%~30%甲醇);流速1.0 ml·min~(-1);柱温40℃;定量离子为m/z 152.1(负离子),多重反应监测。结果:检出限为0.016 ng,线性关系范围0.187~3.749 ng,平均加样回收率为94.3%,RSD为3.19%(n=9)。结论:本法结果准确,便于操作,可用于乌鸡白凤丸中氯霉素的残留量控制。
Objective: To establish a method for the determination of chloramphenicol residue in Wuji Baifeng pills by liquid chromatography tandem mass spectrometry with normal solid-phase extraction. Methods: A normal solid-phase extraction column was used for the sample pretreatment and enrichment,and high performance liquid chromatography tandem mass spectrometry was used to determine chloramphenicol residue in Wuji Baifeng pills. The analysis was performed on an Agilent-ODS C18( 250 mm × 4. 6 mm,5 μm)column. The mobile phase was composed of methanol and water with gradient elution at 40℃( 0-7 min,30% methanol; 7~(-1)5 min,30%-80% methanol; 15-25 min,80%-30% methanol). The flow rate was 1. 0 ml·min~(-1),and the quantitation ion was m/z 152. 1( the negative ionization) under the mode of multiple reaction monitoring. Results: The limit of detection was 0. 016 ng. The calibration curves were linear within the range of 0. 187-3. 749 ng. The method recovery was 94. 3% with RSD of 3. 19%( n = 9). Conclusion: The method is simple with accurate results. It is suitable for the determination of chloramphenicol residue.
Objective: To establish a method for the determination of chloramphenicol residue in Wuji Baifeng pills by liquid chromatography tandem mass spectrometry with normal solid-phase extraction. Methods: A normal solid-phase extraction column was used for the sample pretreatment and enrichment,and high performance liquid chromatography tandem mass spectrometry was used to determine chloramphenicol residue in Wuji Baifeng pills. The analysis was performed on an Agilent-ODS C18( 250 mm × 4. 6 mm,5 μm)column. The mobile phase was composed of methanol and water with gradient elution at 40℃( 0-7 min,30% methanol; 7~(-1)5 min,30%-80% methanol; 15-25 min,80%-30% methanol). The flow rate was 1. 0 ml·min~(-1),and the quantitation ion was m/z 152. 1( the negative ionization) under the mode of multiple reaction monitoring. Results: The limit of detection was 0. 016 ng. The calibration curves were linear within the range of 0. 187-3. 749 ng. The method recovery was 94. 3% with RSD of 3. 19%( n = 9). Conclusion: The method is simple with accurate results. It is suitable for the determination of chloramphenicol residue.
引文
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2 吉文亮,马永建,仓公敖.高效液相色谱串联质谱法测定蜂蜜中残留氯霉素[J].药物分析杂志,2006,26(12):1814-1817
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5 姚令文,陈佳,王钢立,等.UPLC测同仁乌鸡白凤丸中芍药苷含量[J].药物分析杂志,2009,29(9):1522-1524
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8 李博,陈磊,朱韵韵.固相萃取-高效液相色谱法测定牛乳中氯霉素残留[J].中国卫生检验杂志,2005,15(12):1426-1428
9 中国国家标准化委员会.GB/T22338-2008动物源性食品中氯霉素残留量测定[S].2008
2 吉文亮,马永建,仓公敖.高效液相色谱串联质谱法测定蜂蜜中残留氯霉素[J].药物分析杂志,2006,26(12):1814-1817
3 陈小霞,岳振峰,郑卫平,等.液质联用法测定鸡肉组织中氯霉素残留的研究[J].药物分析杂志,2006,26(1):110-114
4 李丽莉,罗轶.液相色谱-串联质谱法测定鸡肉中氯霉素残留[J].中国卫生检验杂志,2011,26(6):1357-1358
5 姚令文,陈佳,王钢立,等.UPLC测同仁乌鸡白凤丸中芍药苷含量[J].药物分析杂志,2009,29(9):1522-1524
6 聂黎行,李向日,金红宇,等.同仁乌鸡白凤丸中重金属和农药残留的测定[J].中国中药杂志,2007,32(23):2563-2567
7 芦艳芬,周莹.固相萃取-高效液相色谱法测定禽畜肉中氯霉素残留[J].中国卫生检验杂志,2008,18(1):57-59
8 李博,陈磊,朱韵韵.固相萃取-高效液相色谱法测定牛乳中氯霉素残留[J].中国卫生检验杂志,2005,15(12):1426-1428
9 中国国家标准化委员会.GB/T22338-2008动物源性食品中氯霉素残留量测定[S].2008