高效液相色谱-串联质谱法同时测定畜禽肉和牛奶中地塞米松和氯丙嗪残留

Simultaneous determination of dexamethasone and chlorpromazine residues in livestock and poultry meat and milk by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  畜禽肉  牛奶  地塞米松  氯丙嗪  高效液相色谱-串联质谱法

英文关键词:livestock and poultry meat  milk  dexamethasone  chlorpromazine  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定畜禽肉和牛奶中地塞米松和氯丙嗪残留的方法。方法 样品经乙腈提取, C18固相分散萃取净化, 以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱, 经C18色谱柱分离, 采用电喷雾正离子(electronic spay ionization, ESI+)模式, 以多反应监测(multiple reaction monitoring, MRM)模式进行分析, 外标法定量。结果 该方法在0.5~200.0 μg/L范围内线性关系良好(r＞0.999), 方法检出限为0.1 μg/kg, 定量限为0.3 μg/kg。在添加水平为0.5、1.0、5.0、10.0、25.0、50.0 μg/kg时, 平均回收率为70.1%~119.4%, 相对标准偏差为1.6%~9.4% (n=6)。结论 该方法简单高效、灵敏度高、重复性好、准确度高, 适用于畜禽肉和牛奶中地塞米松和氯丙嗪残留的同时测定。

英文摘要:

      Objective To establish a methord for the simultaneous determination of the dexamethasone and chlorpromazine residues in livestock and poultry meat and milk by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile, purified by C18 solid phase dispersion extraction, separated on a C18 column by gradient elution with acetronitrile-containing 0.1% formic acid water as mobile phase, analyzd in positive electronic spay ionization (ESI+) mode with dynamic multiple reaction monitoring (MRM), and quantified by the external standard method. Results The linearity of the method was good in the range of 0.5-200.0 μg/L, and the correlation coefficients were greater then 0.999, the limit of detection was 0.1 μg/kg and the limit of quantification was 0.3 μg/kg. The average recoveries were 70.1%-119.4% at the spiked levels of 0.5, 1.0, 5.0, 10.0, 25.0, 50.0 μg/kg, the relative standard deviations were 1.6%-9.4% (n=6). Conclusion This method is simple and efficient, sensitive, reproducible and accurate, which is suitable for the determination of dexamethasone and chlorpromazine residues in livestock and poultry meat and milk.