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目的 :建立大鼠血浆中1-脱氧野尻霉素(DNJ)的液相色谱-质谱联用(LC-MS/MS)测定方法,并用于大鼠口服桑叶总生物碱后DNJ的药代动力学研究。方法 :血浆样品经甲醇沉淀蛋白后,以乙腈-6.5 mmol·L-1甲酸铵水溶液为流动相,采用Agilent Eclipse Plus C18柱(2.1 mm×150 mm,3.5μm)进行分离,梯度洗脱,流速0.4 mL·min-1。采用电喷雾离子源,多反应监测(MRM)模式,正离子检测,用于定量的离子反应为m/z 164.0→69.0(DNJ),m/z 208.1→146.0(米格列醇,内标)。结果 :DNJ在1~500 ng·mL-1浓度范围内线性关系良好,日内、日间精密度(RSD)均小于10.9%,准确度在92.4%~112.7%,DNJ和内标的提取回收率均大于84.1%。结论 :本方法快速、灵敏、操作简便,可用于1-脱氧野尻霉素的药代动力学研究。
OBJECTIVE: To establish a liquid chromatography-mass spectrometry (LC-MS / MS) method for the determination of 1-deoxynojirimycin (DNJ) in rat plasma and to study the pharmacokinetics of DNJ after oral administration of mulberry leaf alkaloids Study. METHODS: Plasma samples were precipitated with methanol and eluted with acetonitrile-6.5 mmol·L-1 ammonium formate aqueous solution using an Agilent Eclipse Plus C18 column (2.1 mm × 150 mm, 3.5 μm) for gradient elution. The flow rate 0.4 mL · min-1. Electrospray ionization, multi-reaction monitoring (MRM) mode and positive ion detection were used to quantify the ion reaction for m / z 164.0 → 69.0 (DNJ), m / z 208.1 → 146.0 (miglitol, internal standard) . Results: The linearity of DNJ was within the range of 1 ng / mL to 500 ng · mL-1. The intra-day and inter-day RSD were less than 10.9% and the accuracy was between 92.4% and 112.7%. The recoveries of DNJ and internal standard Greater than 84.1%. Conclusion: The method is rapid, sensitive and easy to operate. It can be used to study the pharmacokinetics of 1-deoxynojirimycin.