【摘要】 建立超高效液相色谱-串联质谱法测定八宝粥罐头中乙二胺四乙酸二钠(ethylenediaminetetraacetic acid disodium,EDTA-2Na)残留量的检测和确证方法。试样中残留的EDTA-2Na用水高速匀浆提取,提取液经三氯化铁衍生化、三氯甲烷和MAX阴离子交换柱净化后,用超高效液相色谱-串联质谱仪检测和确证,外标法定量。EDTA-2Na质量浓度在1.0~50.0 μg/m L范围内时,线性关系良好,EDTA-2Na的相关系数(R2)为0.992 2。在20~400 mg/kg添加范围内,样品平均加标回收率在79.4%~105.3%之间,相对标准偏差为7.93%~9.94%。EDTA-2Na的最低检出限为20 mg/kg。该方法具有灵敏、准确、稳定等优点,可用于八宝粥罐头中EDTA-2Na残留量测定。更多还原

【Abstract】 An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) method was developed for the determination and confirmation of ethylenediaminetetraacetic acid disodium(EDTA-2Na) residues in canned eight-ingredient porridge. The EDTA-2Na residues in the test samples were extracted with water by means of high-speed homogenization. The extract was derivatized with Fe Cl3 reagent, cleaned up by chloroform and MAX anion exchange column. The residues were determined and confirmed by UPLC-MS-MS using an external standard method. The linear range was 1.0–50.0 μg/m L for EDTA-2Na with a correlation coefficient(R2) of 0.992 2. The average recoveries of EDTA-2Na in spiked samples ranged from 79.4%–105.3%, with relative standard deviations between 7.93% and 9.94% at spiked levels of 20–400 mg/kg. The limit of detection was 20 mg/kg for EDTA-2Na. The method is sensitive, accurate, repeatable and suitable for the determination of EDTA-2Na residues in canned eight-ingredient porridge.更多还原