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目的建立高效液相色谱-质谱/质谱(HPLC-MS/MS)测定盐酸苯乙双胍及片剂中有关物质双氰胺含量的方法。方法色谱条件:采用Agilent Eclipse XDB-C18色谱柱(4.6mm×150mm,3.5μm),以甲醇-0.1%甲酸溶液(30:70)为流动相;流速:0.5mL.min-1;柱温:30℃;质谱条件:采用大气压化学电离(APCI)源进行正离子检测,选择离子监测(SRM)方式定量分析,双氰胺和内标盐酸苯丙醇胺的监测离子对分别为m/z85→68和m/z152→134。结果 HPLC-MS/MS测定盐酸苯乙双胍中双氰胺含量的线性范围为0.001～10.41μg.mL-1(r=0.9999);加样回收率平均值达98.0%,RSD为1.8%;中间精密度的RSD为5.3%;重复性的RSD为1.9%。结论本法灵敏度高、专属性强、简便、快速、准确,适用于盐酸苯乙双胍及片剂中双氰胺的定量测定。
Objective To develop a HPLC-MS / MS method for the determination of dicyandiamide in the phenformin hydrochloride and tablets. Method Chromatographic conditions: Agilent Eclipse XDB-C18 column (4.6mm × 150mm, 3.5μm) with methanol-0.1% formic acid solution (30:70) as mobile phase; flow rate: 0.5mL · min -1; 30 ℃; Mass spectrometry conditions: positive ion detection with atmospheric pressure chemical ionization (APCI) source and quantitative ion selective ion monitoring (SRM) mode. The monitored ion pairs of dicyandiamide and internal standard phenylpropanolamine hydrochloride are m / z85 → 68 and m / z 152 → 134. Results The linear range of dicyandiamide in phenformin hydrochloride was 0.001 ~ 10.41μg.mL-1 (r = 0.9999) by HPLC-MS / MS. The average recoveries were 98.0% with RSD of 1.8% The RSD of precision was 5.3%; the repeatability RSD was 1.9%. Conclusion This method has high sensitivity, specificity, and is simple, rapid and accurate. It is suitable for the quantitative determination of dicyandiamide in phenformin hydrochloride and tablets.