超高效液相色谱-串联质谱法快速测定镇咳祛痰药中阿片类物质的含量

建立了镇咳祛痰药中吗啡、可待因、海洛因、蒂巴因、罂粟碱、那可汀6种阿片类物质含量的LCM S/M S快速测定方法。药品经超声浸取,甲醇稀释过滤后经Waters C₁₈柱分离,以乙腈和10 mmol/L乙酸铵(含0.1%甲酸)溶液进行梯度洗脱,采用电喷雾正离子化(ESI+)、多反应监测模式进行测定。6种阿片类物质在相应的线性范围内线性均良好(r> 0.9995),检出限为吗啡0.2 ng/mL、可待因0.1 ng/mL、海洛因0.03 ng/mL、蒂巴因0.07 ng/mL、罂粟碱0.002 ng/mL、那可汀0.001 ng/mL。日内精密度为0.89%~2.5%,日间精密度为1.5%~5.5%,加标回收率在77.7%~90.5%之间。方法适用于镇咳祛痰药中吗啡、可待因、海洛因、蒂巴因、罂粟碱、那可汀6种阿片类物质的定性定量检测及质量控制。

Rapid determination of opioids in antitussive and expectorant drugs by ultra performance liquid chromatography-tandem mass spectrometry

A rapid ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of morphine,codeine,heroin,thebaine,papaverine and narcotine in antitussive and expectorant drugs.The drugs were leached by ultrasonication,diluted with methanol and filtered,and then separated by Waters C₁₈ column.A gradient elution of acetonitrile and 10 mmol/L ammonium acetate(containing 0.1% formic acid) was carried out,and electrospray positive ionization(ESI+) and multiple reaction monitoring mode was employed for MS/MS detection.Good linear ranges of six opioids were obtained with the correlation coefficients of above 0.9995.The detection limits were 0.2,0.1,0.03,0.07,0.002 and0.001 ng/m L for morphine,codeine,heroin,tiabain,papaverine and narcotine,respectively.The intra-day relative standard deviations were 0.89%-2.5%,the inter-day relative standard deviations of opioids were1.5%-5.5%,and the average recoveries ranged from 77.7% to 90.5%.The method is suitable for the qualitative and quantitative determination of 6 opioids in morphine,codeine,heroin,thebaine,papaverine and narcotine.