高效液相色谱-串联质谱法测定中药中桔青霉素

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2.5 μg·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 sensitive and accurate method for the determination of citrinin in traditional Chinese medicine by LC-MS/MS. Methods: Citrinin in traditional Chinese medicines was extracted by 70% methanol, and then purified by immunoaffinity columns. The mass spectrometer was operated in the positive ionization electrospray(ESI) mode using multiple reaction monitoring(MRM) for analysis of citrinin. The transitions m/z 251→233 and m/z 472→436 were used to quantify citrinin and terfenadine(internal standard), respectively. Results: The method had satisfactory linearity in the range of 0.1-50 ng·mL^-1 with a regression coefficient of 0.9994, the intra-and inter-day RSDs were both below 5.4%, the limit of quantification(LOQ) was 2.5 μg·kg^-1, and the mean recoveries ranged from 81.2% to 93.3%. Conclusion: The method is sensitive, simple and accurate, and proved to be suitable in the determination of citrinin in the complicated traditional Chinese medicine matrices.