| 超高效液相色谱―串联质谱法检测猪肝中乙酰异戊酰泰乐菌素残留 |
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| 引用本文： | 王莹,张素霞,程林丽,刘凯丽.超高效液相色谱―串联质谱法检测猪肝中乙酰异戊酰泰乐菌素残留[J].中国畜牧兽医,2011,38(10):224-227. |
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| 作者姓名： | 王莹 张素霞 程林丽 刘凯丽 |
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| 作者单位： | 中国农业大学动物医学院,北京 100193 |
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| 基金项目： | 农业行业标准(2010) |
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| 摘 要： | 本研究建立了猪肝中乙酰异戊酰泰乐菌素残留的超高效液相色谱―串联质谱检测方法(UPLC-MS/MS)。样品经EDTA-McIlvaine's缓冲液提取,HLB固相萃取柱净化后,采用C18色谱柱分离,以乙腈―0.1％甲酸(7∶3,V/V)为流动相洗脱,电喷雾正离子模式电离,选择离子监测模式检测。结果表明,药物浓度与峰面积在5~2000 ng/mL范围内呈现良好的线性关系,相关系数大于0.99,对空白猪肝组织进行5~500 μg/kg的药物添加回收试验,经统计分析获得平均回收率约为84.9%~88.1%,批内变异系数为8.2％~15.1%,批间变异系数为14.7％~16.5%。本方法对乙酰异戊酰泰乐菌素的检测限为0.76 μg/kg,定量限为2.51 μg/kg,方法灵敏、准确,适用于猪肝脏中乙酰异戊酰泰乐菌素残留的检测。
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| 关 键 词： | 超高效液相色谱―串联质谱法 猪肝 乙酰异戊酰泰乐菌素 残留 |
| 收稿时间： | 2011-03-07 |
Determination of Residue Acetylisovaleryltylosin in Swine Liver by UPLC-MS/MS |
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| WANG Ying,ZHANG Su-xia,CHENG Lin-li,LIU Kai-li.Determination of Residue Acetylisovaleryltylosin in Swine Liver by UPLC-MS/MS[J].China Animal Husbandry & Veterinary Medicine,2011,38(10):224-227. |
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| Authors: | WANG Ying ZHANG Su-xia CHENG Lin-li LIU Kai-li |
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| Institution: | College of Veterinary Medicine,China Agricultural University,Beijing 100193, China |
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| Abstract: | An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for determination of acetylisovaleryltylosin in swine liver.The target drug was extracted from sample with EDTA-McIlvaine's and the extract was cleaned up on an Oasis HLB cartridge. Separation was performed on C18 column with acetonitrile-0.1% formic acid(7∶3,V/V) as the mobile phase. The identification of drug was carried out by positive electrospray ionization (ESI+) under selective ion monitoring mode (SIM). The calibration curve of the drug showed excellent linearity within the range of 5 to 2000 ng/mL and the correlation coefficient was more than 0.99. The average recoveries from spiked swine liver at levels of 5 to 500 μg/kg ranged from 84.9% to 88.1%, the intra-day coefficient variation was in range of 8.2% to 15.1% and inter-day coefficient variation was in range of 14.7% to 16.5%. The limit of detection (LOD) was 0.76 μg/kg and limit of quantification (LOQ) was 2.51 μg/kg.The method was accurate and sensitive, so it could be used for determining of acetylisovaleryltylosin in swine liver. |
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| Keywords: | UPLC-MS/MS swine liver acetylisovaleryltylosin residue |
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