QuEChERS结合UHPLC-MS/MS测定火锅汤料中禁用染料及罂粟壳

Determination of Industrial Dyes and Papaveris pericarpium in Hot Pot Soup Seasoning by QuEChERS-UHPLC-MS/MS

为建立同时测定火锅汤料中5种禁用染料(苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、罗丹明B)及罂粟壳生物碱(吗啡、可待因、蒂巴因、罂粟碱、那可丁)的QuEChERS-超高效液相色谱-串联质谱方法,样品采用乙腈提取,无水硫酸镁-无水乙酸钠盐析,乙二胺-N-丙基硅烷(PSA)进行净化处理。液相色谱以C18柱为分析柱,乙腈-10 mmol/L乙酸铵溶液作为流动相体系进行梯度洗脱。质谱分析采用电喷雾正离子、多反应监测扫描模式(MRM),基质匹配标准曲线,外标法定量。各目标物在各自浓度范围内线性良好,在三个水平进行加标回收试验,回收率在71.6%~94.1%之间,相对标准偏差(RSD)在2.4%~8.9%之间,方法检出限为0.5~10μg/kg。该方法具有操作简单、准确、灵敏度高等优点,适合批量样品的快速测定。

A new method for the simultaneous determination of five industrial dyes(Sudan red Ⅰ, Sudan red Ⅱ, Sudan red Ⅲ, Sudan red Ⅳ and Rhodamine B) and Papaveris pericarpium(Morphine, codeine, thebaine, papaverine and narcotine) in hot pot soup seasoning was developed by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The analytes were extracted with acetonitrile, salted out with anhydrous magnesium-anhydrous sodium acetate, and then purified with primary secondary amine(PSA). Chromatographic analysis was carried out C18 column using a mobile phase comprised of acetonitrile-10 mmol/L ammonium acetate in gradient program. The analytes were analyzed by positive electrospray ionization tandem mass spectrometry under multiple reaction monitoring(MRM) mode. Quantification was achieved using matrix-matched external standard method. The calibration curves showed a good linearity in each concentration range. The recoveries of three spiking levels ranged from 71.6% and 94.1%, the relative standard deviation(RSD) was between 2.4% and 8.9%, and the limits of detection were in the range of 0.5 μg/kg to10 μg/kg. The method was simple, accurate and sensitive, and it was suitable for the rapid determination of the batch of samples.