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目的:建立测定中药中桔青霉素含量的高效液相色谱-串联质谱法,对市售中药材及其制品中的桔青霉素进行检测。方法:样品用70%甲醇提取,经免疫亲和柱净化,采用高效液相色谱-串联质谱法测定其中桔青霉素的含量,采用多反应监测(MRM)方式分别监测离子对m/z 251→233(桔青霉素)和m/z 472→m/z 436(内标特非那定)。结果:以桔青霉素和内标特非那定峰面积的比值对桔青霉素的浓度作线性回归,桔青霉素浓度在0.1～50 ng.mL-1范围内线性关系良好(r=0.9994),日内和日间精密度以RSD表示均低于5.4%,方法的定量限为2.5μg.kg-1,平均回收率在81.2%～93.3%的范围内。结论:该方法快速、灵敏,结果准确,适用于复杂中药基质中桔青霉素的检测。
Objective: To establish a method for the determination of citrinin in traditional Chinese medicine by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods: The samples were extracted with 70% methanol and purified by immunoaffinity column. The contents of citrinin were determined by high performance liquid chromatography-tandem mass spectrometry. The m / z 251 → 233 (Citrinin) and m / z 472 → m / z 436 (terfenadine as internal standard). Results: The linear regression was obtained for the concentration of citrinin with the ratio of peak areas of citrinin and terfenadine. There was a good linear relationship between the concentration of citrinin and 0.1 ~ 50 ng.mL-1 (r = 0.9994) Inter-precision RSD less than 5.4%, the limit of quantification of 2.5μg.kg-1, the average recovery was in the range of 81.2% to 93.3%. Conclusion: The method is rapid, sensitive and accurate. It is suitable for the detection of citrinin in the complex traditional Chinese medicine matrix.