摘要
目的建立超高效液相色谱-串联质谱法测定复合调味酱产品中乙基麦芽酚的含量的分析方法。方法样品用水分散均匀后,用乙腈提取其中的乙基麦芽酚,加入氯化钠盐析处理,离心后,上清液经正己烷和混合净化粉末(1 g无水硫酸镁、0.1 g石墨化碳黑粉末、0.2 g乙二胺-N-丙基硅胶(primary secondary amine, PSA)粉末和0.2 g C18粉末)进行脱脂、脱色和净化处理后,由C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行等度洗脱,采用正离子多反应离子检测模式对乙基麦芽酚进行检测,外标法定量。结果乙基麦芽酚含量在10~500ng/mL(0.04~2.0mg/kg)范围内线性关系良好,相关系数大于0.99,检出限为0.01mg/kg,定量限均为0.04 mg/kg,加标回收率为89.3%~99.3%,相对标准偏差为1.4%~2.6%。结论该方法可用于复合调味酱产品中乙基麦芽酚含量的测定,能够为在复合调味酱产品中乙基麦芽酚暴露量数据累积提供技术支持。
Objective To establish a method for the determination of ethyl maltophenol in compound flavor sauce products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was firstly dispersed with water, and extracted with acetonitrile. Sodium chloride was added and centrifuged in order to salting out to obtain the organic layer. Then the supernatant was degreased, decolorized and cleaned with n-hexane and mixed cleanup powder(compounded with 1 g anhydrous magnesium sulfate, 0.1 g graphitized carbon powder, 0.2 g PSA powder and 0.2 g C18 powder), separated by C18 column using acetonitrile and 0.1% formic acid aqueous solution as the mobile phase for isocratic elution, ethyl maltol was detected by positive ion multi-reactive ion detection mode, and quantified by external standard method. Results The content of ethyl maltol had a good linear relationship within the range of 10~500 ng/mL(0.04–2.0 mg/kg), and the correlation coefficient was greater than 0.99. The limit of detection was 0.01 mg/kg, and the limit of quantification was 0.04 mg/kg. The standard recovery rates were 89.3%–99.3%, and the relative standard deviations were 1.4%–2.6%. Conclusion This method can be used for the determination of ethyl maltol content in compound seasoning sauce products, and can provide technical support for the accumulation of ethyl maltol exposure data in compound seasoning sauce products.
作者
郭建博
刘开
宋莉
薛晓文
王蕊
林芳
王晶
李涛
GUO Jian-Bo;LIU Kai;SONG Li;XUE Xiao-Wen;WANG Rui;LIN Fang;WANG Jing;LI Tao(Shaanxi Institute for Food and Drug Control,Xi’an 710065,China)
出处
《食品安全质量检测学报》
CAS
2020年第19期6745-6750,共6页
Journal of Food Safety and Quality
基金
陕西省重点产业链(群)项目(2019ZDLSF07-08)
陕西省创新能力支撑计划项目(2019PT-22)。
关键词
乙基麦芽酚
复合调味酱
超高效液相色谱-串联质谱法
ethyl maltol
compound flavor sauce products
ultra performance liquid chromatography tandem mass spectrometry
