Determination of 14 nonsteroidal anti-inflammatory drugs by molecularly imprinted polymers solid phase extraction with ultra-high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了一种基于分子印迹固相萃取-超高效液相色谱串联质谱法测定猪肉及猪肝中14种非甾体抗炎药的测定方法。样品经10 mmol/L p H3.0甲酸铵缓冲液提取2次,合并提取液经正己烷除脂后,使用分子印迹固相萃取柱进行净化。待测化合物经BEH C18色谱柱分离,以乙腈-5 mmol/L乙酸铵水溶液（含0.1%甲酸）进行梯度洗脱,电喷雾电离,正负离子切换模式下使用多反应监测扫描,基质加标曲线定量。14种非甾体抗炎药在0.2550μg/L的范围内线性关系良好,检出限和定量限分别为0.12μg/kg和0.255μg/kg。在猪肉、猪肝中的3个添加水平下,平均回收率为73.2%110.7%,相对标准偏差1.0%9.7%。该方法灵敏度、精密度、准确性均满足兽药残留检测的要求,适用于非甾体抗炎药多组分残留检测。Abstract: A molecularly imprinted solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry method was established for the determination of 14 kinds of nonsteroidal anti-inflammatory drugs in pork and liver. Sample was extracted twice by 10 mmol/L p H3.0 ammonium formate buffer, followed with defat by n-hexane.Supernatant was purified by molecularly imprinted solid phase extraction. Analytes were separated by BEH C18 column under gradient elution, then detected with mass spectrometry under positive and negative electric spray ionization and multiple reactions monitoring mode. The calibration curves of 14 nonsteroidal anti-inflammatory drugs were linear in the range of0.2550 μg/L. The limits of detection and quantitation were 0.1 ~ 2 μg/kg and 0.25 ~ 5 μg/kg, respectively. In three different spike levels, the average recoveries in pork and liver were between 73.2% ~ 110.7%, with relative standard deviations of1.0% 9.7%. The sensitivity, precision and accuracy of this method were in accordance with the demand of veterinary residue determination, it is suitable for the multi residue determination of nonsteroidal anti-inflammatory drugs.
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