UHPLC-MS/MS同时测定中药饮片中4种恩镰孢菌素

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

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,2.7μm)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0.002~0.02μg·kg^(-1),定量限为0.01~0.1μg·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。

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,2.7μm)using the mobile phase of 2 mmol·L^(-1) ammonium 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 0.02μg·kg^(-1) and from 0.01 to 0.1μg·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.