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目的:建立液相色谱-质谱联用(LC-MS/MS)方法测定不同产地桑叶中1-脱氧野尻霉素(DNJ)的含量。方法:采用Waters Atlantis Hilic Silica柱(2.1 mm×100 mm,3μm),流动相:乙腈-0.4%醋酸水溶液(80∶20,v/v),等度洗脱,流速为0.4 m L/min,柱温30℃。采用电喷雾离子源(ESI源),多反应监测(MRM)模式,正离子检测,DNJ定量离子对为m/z 164.0→69.0。结果:DNJ在20~1000 ng(r=0.9997)范围内线性关系良好,平均回收率为91.7%。不同产地桑叶中DNJ的含量有较大差异,含量在0.05%~0.50%,四川产地的DNJ含量较高,达到0.50%,亳州产地含量较低,仅为0.05%。结论:该方法操作简单,分析快速,为桑叶药材中1-脱氧野尻霉素的质量控制提供了参考。
Objective: To establish a method for the determination of 1-deoxynojirimycin (DNJ) in mulberry leaves from different habitats by liquid chromatography-mass spectrometry (LC-MS / MS). METHODS: Waters Atlantis Hilic Silica column (2.1 mm × 100 mm, 3 μm) was used. The mobile phase consisted of acetonitrile-0.4% aqueous acetic acid (80:20 v / v) Column temperature 30 ℃. Electrospray ionization (ESI source), multi-reaction monitoring (MRM) mode and positive ion detection were used. The ion pair of DNJ was m / z 164.0 → 69.0. Results: DNJ had good linearity in the range of 20-1000 ng (r = 0.9997) with an average recovery of 91.7%. The contents of DNJ in mulberry leaves of different habitats are quite different, ranging from 0.05% to 0.50%. The content of DNJ in Sichuan origin is relatively high, reaching 0.50%. The content of origin in Bozhou is low, only 0.05%. Conclusion: The method is simple, rapid analysis, and provides a reference for the quality control of 1-deoxynojirimycin in mulberry leaves.