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目的建立简便、快速、灵敏的液相色谱-串联质谱法(LC-MS/MS)同时测定雷公藤饮片中雷公藤甲素、雷公藤红素、雷公藤内酯酮和雷公藤内酯甲的含量,为雷公藤饮片的质量控制与临床应用提供依据。方法采用液相色谱质谱联用技术。色谱条件:Agilent ZORBAX Eclipse Plus C18(2.1 mm×150 mm,3.5μm)色谱柱,乙腈-0.1%甲酸水为流动相进行梯度洗脱,流速为0.2 mL·min~(-1),柱温为35℃;采用电喷雾离子源(ESI),以正离子多反应监测模式进行检测,检测成分的离子对质荷比分别为:雷公藤甲素(361.1/145.1)、雷公藤内酯酮(358.9/143)、雷公藤红素(451.2/201.1)、雷公藤内酯甲(455.3/409.2)。结果雷公藤甲素、雷公藤内酯酮、雷公藤红素和雷公藤内酯甲分别在100~3000 ng·mL~(-1)、100~3000 ng·mL~(-1)、20~600 ng·mL~(-1)和50~1000 ng·mL~(-1)的浓度范围内,线性关系良好(r>0.999)。平均回收率为100.45%~102.74%,其RSD<3.15(n=6)。结论本研究所建立的LC-MS/MS色谱法稳定可靠、简便易行,可同时检测雷公藤饮片中雷公藤甲素、雷公藤红素、雷公藤内酯酮、雷公藤内酯甲4种萜类成分的含量,可为雷公藤饮片及雷公藤制剂的质量控制提供科学依据。不同地区的雷公藤饮片成分含量差异明显。
Objective To establish a simple, rapid and sensitive LC-MS / MS method for the simultaneous determination of triptolide, tripterine, triptolide and triptolide in Tripterygium wilfordii Tablets. Provide the basis for quality control and clinical application of Tripterygium wilfordii Pieces. Methods Using liquid chromatography-mass spectrometry. Chromatographic conditions: a gradient elution was performed on an Agilent ZORBAX Eclipse Plus C18 (2.1 mm × 150 mm, 3.5 μm) column with acetonitrile-0.1% formic acid as mobile phase at a flow rate of 0.2 mL · min -1 with a column temperature of 35 ℃. The ion-pair mass-to-charge ratios of test components were as follows: triptolide (361.1 / 145.1), triptolide (358.9 / 143), electrospray ionization (ESI) ), Tripterine (451.2 / 201.1), triptolide A (455.3 / 409.2). Results Triptolide, triptolide, triptolide and triptolide were in the range of 100 ~ 3000 ng · mL -1, 100 ~ 3000 ng · mL -1, 20 ~ 600 ng · ML -1 and 50-1000 ng · mL -1, the linearity was good (r> 0.999). The average recoveries ranged from 100.45% to 102.74% with RSD <3.15 (n = 6). Conclusion The LC-MS / MS method established in this study is stable, reliable and simple. It can detect triptolide of triptolide, tripton, triptolide and triptolide triptolide simultaneously The content of the ingredients can provide the scientific basis for the quality control of Tripterygium tablets and Tripterygium preparations. Different regions of Tripterygium Pieces significant differences in the content of ingredients.