不同前处理方法对食品中罂粟壳检测效果对比

采用高效液相色谱-三重四极杆质谱联用法作为检测方法,通过对比QuEChERS法和固相萃取法(Oasis PRiME HLB和Oasis MCX)对不同食品基质火锅底料、辣椒粉和肉汤中5种生物碱检测效果的影响,优选食品中罂粟壳检测的普适性前处理方法。结果表明:5种生物碱中罂粟碱、那可丁、蒂巴因在0.2~10 μg/L,可待因、吗啡在1~50 μg/L的浓度范围内呈现出良好的线性关系,决定系数(R2)均大于0.9994;采用QuEChERS法和固相萃取法(Oasis PRiME HLB和Oasis MCX)分别对样品进行前处理后,测得的基质效应分别为0.12%~0.44%,0.02%~0.82%,0.07%~0.41%,检出限分别为0.1~5.0、0.1~8.0、0.1~5.0 μg/kg;回收率和相对标准偏差(RSDs)分别为70.6%~105.3%,64.2%~116.9%,73.6%~102.5%和2.0%~8.5%,1.6%~8.3%,1.6%~7.8%(n=6)。同时本研究对50批次市售火锅底料、辣椒粉、肉汤等样品进行检测,发现1批次石锅鸡汤含有那可丁、罂粟碱、蒂巴因和吗啡4种生物碱,所检出的生物碱成分与高效液相色谱-四极杆-飞行时间质谱仪的一级质谱匹配度良好。因此,固相萃取法(Oasis MCX)更适用于食品中罂粟壳检测的提取和净化,能够满足对不同基质食品中罂粟壳的定性、定量分析。

Comparison of Different Sample Pretreatments for the Analysis of Poppy Husk in Food

High performance liquid chromatography-triple quadrupole mass spectrometer(HPLC-MS/MS)was applied to compare the QuEChERS method and solid phase extraction(Oasis PRiME HLB and Oasis MCX)on the assay of five alkaloids in hot pot sauce,chilli powder and soup.A general pretreatment method of poppy husk was optimized. The results showed that a good linear relationship in the ranges of 0.2~10 μg/L for papaverine,noscapine and thebaine,1~50 μg/L for codeine and morphine with coefficient of determination(R2)greater than 0.9994. The matrix effects of the three pretreatments(QuEChERS,PRiME HLB,Oasis MCX)were 0.12%~0.44%,0.02%~0.82%,0.07%~0.41%,respectively. The limits of detection were 0.1~5.0,0.1~8.0,0.1~5.0 μg/kg. The average recoveries were in the range of 70.6%~105.3%,64.2%~116.9%,73.6%~102.5% and the relative standard deviations(RSDs)were 2.0%~8.5%,1.6%~8.3%,1.6%~7.8%(n=6). The method of Oasis MCX was more suitable for the extraction and purification of poppy husk in food which were applied to 50 batches of hot pot sauce,chilli powder and soup with high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(HPLC-Q-TOF/MS)verifying the reliability of the results.Noscapine,papaverine,thebaine and morphine were detected in a positive sample of chicken soup which was consistent with the result of the first-order mass spectra of HPLC-Q-TOF/MS. Therefore,the method of Oasis MCX can satisfy the qualitative and quantitative analysis of poppy husk in different food.