超高效液相色谱-串联质谱法检测汤料食品中罂粟壳成分

Determination of poppy shell in soup foods by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  汤料食品  罂粟壳

英文关键词:ultra performance liquid chromatography tandem mass spectrometry  soup foods  poppy shell

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)定性定量检测市售麻辣烫、火锅底料及牛肉汤等汤料食品中罂粟碱、吗啡、可待因、那可丁和蒂巴因的分析方法。方法 样品经0.1 mol/L HCl提取、混合阳离子(mixed-cation, MCX)固相萃取柱净化。选用Waters BEH HILIC(2.1 mm×100 mm, 1.7 μm)色谱柱进行分离, 以0.1%(V/V)甲酸-乙腈和0.1%甲酸-10 mmol/L甲酸铵溶液为流动相, 进行梯度洗脱。采用正离子源模式(positive electrospray ionization, ESI+)和多反应检测(multi reaction monitor, MRM)模式进行检测, 内标法定量。结果 在0.1~20 μg/L(吗啡和可待因)以及0.1~4.0 μg/L(蒂巴因、那可丁和罂粟碱)的浓度范围内, 5种罂粟壳物质线性良好, 相关系数均大于0.995, 检出限为0.1~0.5 μg/L, 方法回收率的范围在77.9%~95.5%之间, 相对标准偏差1.75%~9.49%(n=6)。结论 方法简单易行可操作, 且精密度及准确度均较高, 适用于汤料食品中罂粟壳的检测。

英文摘要:

      Objective To establish a qualitative and quantitative method for the determination of papaverine, morphine, codeine, narcotine and thebaine in soup foods such as spicy hot pot, hot pot soup and beef soup by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with 0.1 mol/L HCl, and purified through a mixed-cation (MCX) solid-phase extraction column. Waters BEH HILIC (2.1 mm×100 mm, 1.7 μm) was selected for separation, with 0.1% formic acid (V/V)-acetonitrile and 0.1% formic acid-10 mmol/L ammonium formate solution as mobile phases to carry out gradient elution. Positive electrospray ionization (ESI+) and multiple reaction monitor (MRM) mode were used for determination. The quantification was performed by the internal standard method. Results In the concentration range of 0.1-20 μg/L (morphine and codeine) and 0.1–4.0 μg/L (tibaine, nacodin and papaverine), the linear relation of 5 kinds of poppy shell was well, with all the correlation coefficients over 0.995. The limits of detection were 0.1–0.5 μg/L. The recovery rate of the method ranged from 77.9% to 95.5%, and the relative standard deviation was 1.75%–9.49% (n=6). Conclusion This method is simple, easy to operate and has high precision and accuracy, which is suitable for the detection of poppy shell in soup food.