UHPLC-MS/MS同时测定中药饮片中4种恩镰孢菌素

目的 建立超高效液相色谱-串联质谱法（UHPLC-MS/MS）检测中药饮片中4种恩镰孢菌素含量的分析方法。方法 样品采用70%甲醇超声处理后，以2 mmol·L^–1醋酸铵、甲醇-乙腈为流动相，经Agilent Infinity Lab Poroshell 120 SB-C₁₈色谱柱（2.1 mm×100 mm，2.7 μm）梯度洗脱分离，在电喷雾电离（electrospray ionization，ESI）正离子模式下采用多反应监测（multiple reaction monitoring，MRM）进行测定，基质外标法定量。结果 在高、中、低3个加标水平下，4种恩镰孢菌素的平均回收率为92.15%~118.67%，各恩镰孢菌素在线性范围内线性关系良好，相关系数均≥0.999，方法检出限为0.002~0.02 μg·kg^–1，定量限为0.01~0.1 μg·kg^–1，结果显示4种恩镰孢菌素对17种样品均有不同程度的污染。结论 该方法简便、快速、准确，适用于中药饮片中4种恩镰孢菌素筛查。药饮片中恩镰孢菌素检出率较高。

Simultaneous Determination of 4 Enniatins in Chinese Herbal Slices by UHPLC-MS/MS

OBJECTIVE To establish a method for the simultaneous determination of 4 enniatins in Chinese herbal slices with ultra-high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS). METHODS Samples were extracted with 70% methanol by ultrasound, and the separation of the analytes was carried out on the Agilent Infinity Lab Poroshell 120 SB-C₁₈ column(2.1 mm×100 mm, 2.7 μm) using the mobile phase of 2 mmol·L^-1ammonium acetate and methanol-acetonitrile by gradient elution. The detection was performed in the electrospray ionization(ESI) positive mode and multiple reaction monitoring (MRM) mode, and the matrix-matched calibrations were used to quantify the residue concentrations. RESULTS Satisfactory recoveries of 4 enniatins at low, medium and high spiked levels were ranged from 92.15% to 118.67%. Good linear relationships were obtained and the correlation coefficients(r) were ≥ 0.999, and the limits of detection and quantification ranged from 0.002 to 0.02 μg·kg^-1 and from 0.01 to 0.1 μg·kg^-1 respectively. The results showed that 4 enniatins had different degress of pollution on 17 samples. CONCLUSION The proposed method which is applicative for screening 4 kinds of enniatins is simple, rapid and accurate, and the detection rate is high in Chinese herbal slices.