液相色谱-串联质谱快速检测禽类组织中 黄霉素A残留量
目的 建立检测禽类组织(肌肉、脂肪、肝脏、肾脏)中黄霉素A残留的超快速液相色谱-四极杆/线性离子阱质谱方法。方法 混合均匀的试样经10%氨化甲醇提取, 乙腈沉降蛋白净化后, 以0.3%甲酸-5%乙腈-水溶液和0.3%甲酸?5%水-乙腈为流动相, 使用Agilent Poroshell 120 SB-C18(100 mm×2.1 mm, 2.7 μm)色谱柱超快速液相色谱分离, 优化多反应检测(selected multiple reaction monitoring, sMRM)模式检测, 外标法定量。结果 黄霉素A在20~200 μg/L线性范围内线性关系良好(r≥0.995); 黄霉素A定量限(limit of quantity, LOQ, S/N≥10)为10 μg/kg; 3个添加水平(10、20 和100 μg/kg)下的回收率为66.5%~89.4%; 相对标准偏差(relative standard deviation, RSD)为4.7%~10.2%。结论 该方法快速、准确、灵敏, 可有效用于禽类组织中黄霉素A残留的测定。
Objective To establish a highly sensitive method to confirm moenomycin A residues in poultry tissues (muscle, fat, liver and kidney) by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The poultry tissues were extracted with 10% ammoniation of methanol, and purified by acetonitrile. The chromatography separation was conducted on an Agilent Poroshell 120 SB-C18 column (100 mm×2.1 mm, 2.7 μm) with a mobile phase of 0.3% formic acid-5% acetonitrile–water (v:v:v) and 0.3% formic acid-5% water-acetonitrile (v:v:v) with gradient elution. The analytes were separated by LC and determined by LC-MS/MS and multiple reaction monitor (selected multiple reaction monitoring, sMRM) mode. External standard was used for the quantification. Results Moenomycin A showed a good linearity with the correlation coefficients (r) no less than 0.995 in the range of 20~200 μg/L, with the limits of quantification (limit of quantity, LOQ, S/N≥10) of 10 μg/kg for all analytes. The developed method gave average recoveries of 66.5%~89.4% for drugs spiked at 10~100 μg/kg, with the relative standard deviation of 4.7%~10.2%. Conclusion The proposed method could be used to screen and confirm moenomycin A in a single run, which made it effective in residue surveillance and detection of moenomycin A in poultry tissues.
标题：液相色谱-串联质谱快速检测禽类组织中 黄霉素A残留量
英文标题：Determination of moenomycin A residues in poultry tissues by liquid chromatography-tandem mass spectrometry
作者：
许辉 山东出入境检验检疫局
张鸿伟 山东出入境检验检疫局
王凤美 山东出入境检验检疫局
张晓梅 山东出入境检验检疫局
蔡雪 山东出入境检验检疫局
中文关键词:黄霉素A,液相色谱-串联质谱法,禽类组织,
英文关键词:moenomycin A,liquid chromatography-tandem mass spectrometry,poultry tissues,
发表日期：2014-11-12
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