高效液相色谱-串联质谱法测定药酒中5种罂粟壳生物碱

Determination of 5 opium poppy husk alkaloids in medicinal liquor by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  药酒  高效液相色谱-串联质谱法  罂粟壳生物碱

英文关键词:medicinal liquor  high performance liquid chromatography-tandem mass spectrometry  opium poppy husk alkaloids

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定药酒中非法添加吗啡、可待因、蒂巴因、罂粟碱和那可丁５种罂粟壳生物碱的分析方法。方法 药酒在60 ℃水浴锅中挥去乙醇, 再加入含0.2%(V/V)甲酸的乙腈溶液提取, 最后用分散固相萃取(dispersive solid phase extraction, d-SPE)纯化管净化待测。以乙腈和10 mmol/L乙酸铵溶液(含0.1%甲酸)作为流动相进行梯度洗脱, 选用色谱柱为XtimateTM C18柱, 在0.4 mL/min流速下, 质谱采用电喷雾电离源正离子扫描, 多反应监测模式检测。结果 吗啡和可待因线性范围为5.0~250.0 ng/mL, 蒂巴因、罂粟碱、那可丁的线性范围为1.0~50.0 ng/mL, 相关系数均在0.997以上。5种生物碱的方法检出限和定量限分别为0.02～0.80 μg/L和0.07～3.00 μg/L, 回收率范围为80.3%～101.5%, 相对标准偏差(relative standard deviation, RSD)在3.2%～8.1%之间(n=6)。结论 该方法简便、快速、准确可靠, 可用于药酒中罂粟壳生物碱含量的检测。

英文摘要:

      Objective To establish a method for determination of 5 opium poppy husk alkaloids (papaverine, noscapine, morphine, codeine and thebaine) in medicinal liquor by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods Ethanol in the sample was evaporated by thermostatic water bath at 60 ℃. Residues were extracted by the acetonitrile solution with 0.2%(V/V) formic acid, then purified through dispersive solid phase extraction(dSPE). The separation was carried out using a Xtimate TM C18 column by gradient elution with the mobile phase of acetonitrile and aqueous solution of ammonium acetate (10 mmol/L) containing formic acid (0.1%) as the additive, and detected by mass spectrometry using electrospray ionization (ESI) in positive mode under multiple reaction monitoring mode. Results The linear range for codeine and morphine were 5.0–250.0 ng/mL, and those for papaverine, noscapine and thebaine were 1.0–50.0 ng/mL, with relative coefficients above 0.997. The limits of detection and quantitation were in the range of 0.02–0.80 μg/L and 0.07–3.00 μg/L for the 5 opium poppy husk alkaloids, respectively. The average recoveries of the 5 alkaloids were in the range of 80.3%–101.5%, with relative standard deviation in the range of 3.2%–8.1%(n=6). Conclusion This method is simple, fast, accurate and reliable, which can be used for the determination of five opium poppy husk alkaloids in medicinal liquor.