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目的采用超高效液相色谱-质谱联用方法同时测定复方甘草口服溶液中吗啡、可待因、罂粟碱和可卡因的含量。方法采用Waters BEH C18(50 mm×2.1 mm,1.7μm)色谱柱,流动相为含0.1%甲酸的0.02 mol·L?1乙酸铵溶液(A)-甲醇(B),梯度洗脱(0~1.5 min,92%A;1.5~2.0 min,92%A→60%A;2.0~4.5 min,60%A;4.5~4.6 min,60%A→92%A;4.6~5.0 min,92%A),流速为0.2 m L·min?1,柱温为35℃;质谱采用电喷雾离子源,多反应监测模式(正离子)。结果吗啡、可待因、罂粟碱和可卡因浓度分别在5.68~113.4,1.04~20.85,0.53~10.58和0.16~3.13μg·L?1内线性关系良好,r值为0.998 4~0.999 9,平均回收率为98.8%~100.3%,定量下限分别为0.5,0.5,0.05,0.01μg·L?1,检测限为0.2,0.2,0.02,0.005μg·L?1。结论该方法分析速度快,灵敏度高,结果准确可靠,是复方甘草口服溶液质量控制的一种可行方法。
Objective To determine the contents of morphine, codeine, papaverine and cocaine in compound liquorice oral solution by ultra performance liquid chromatography-mass spectrometry. Methods A Waters BEH C18 (50 mm × 2.1 mm, 1.7 μm) column was used. The mobile phase consisted of 0.02 mol·L -1 ammonium acetate solution (A) with 0.1% formic acid and gradient elution (0 ~ 1.5 to 2.0 min, 92% A to 60% A; 2.0 to 4.5 min, 60% A; 4.5 to 4.6 min, 60% A to 92% A; 4.6 to 5.0 min, 92% A ), The flow rate was 0.2 m L · min -1, and the column temperature was 35 ℃. The mass spectrometry was electrospray ionization source and multi-reaction monitoring mode (positive ion). Results The linearity of morphine, codeine, papaverine and cocaine were 5.68 ~ 113.4, 1.04 ~ 20.85, 0.53 ~ 10.58 and 0.16 ~ 3.13μg · L ~ The rates were from 98.8% to 100.3%. The lower limits of quantitation were 0.5, 0.5, 0.05 and 0.01 μg · L -1, respectively. The limits of detection were 0.2,0.2,0.02,0.005 μg · L -1. Conclusion The method is fast, sensitive and accurate and reliable. It is a feasible method for the quality control of compound liquorice oral solution.