摘要
目的:建立二极管阵列高效液相色谱仪和三重四级杆液质联用仪对豆奶中三聚氰胺的测定方法。方法:采用三氯乙酸和乙腈为提取剂、蛋白质为沉淀剂,提取液过净化柱纯化。结果:三重四级杆液质联用法对三聚氰胺的检出限为0.001 5 mg/kg,标准曲线在0.01~0.5μg/mL范围内,R^2为0.999 8,线性良好,再回收率为85%~89%,适用于检测低浓度的样品;二极管阵列高效液相色谱法检出限为0.024 mg/kg,标准曲线在0.5~100μg/mL范围内,R^2为0.999 9,线性良好,回收率为83%~91%,可以快速地对高浓度样品进行筛查。结论:以上两种检测方法结合使用,可检测0.01~100 mg/kg的三聚氰胺含量,极大地拓宽了检测范围。
【Objective】To establish a method for the melamine in soy milk by HPLC-DAD and LC/MS/MS.【Method】we used trichloroacetic acid and acetonitrile to extract and precipitate impurities.The Extraction was purificated by purification column.【Result】Using LC/MS/MS method,the detection limit was melamine was 0.001 5 mg/kg,the calibration curves showed a good linearity in the range of 0.01~0.5 μg/mL,and the correlation coefficients（R^2） was 0.999 8.The recoveries ranged from 85%~89%.The method was applicable to detect low concentration of sample.While using HPLC-DAD method,the detection limit of melamine was 0.024 mg/kg,the calibration curves showed a good linearity in the range of 0.5~100 μg/mL,and the correlation coefficients（R^2） was 0.999 9.The recoveries ranged from 83%~91%.It was suitable for high concentration of the detection of the sample.【Conclusion】The two kinds of detection methods used in combination could detect 0.01~100 mg/kg of melamine,greatly expand the detection range.
作者
尤妍
YOU Yan(The Inspection Testing Center of Food and Drug in Yuhuan City, Taizhou 317608, China)
出处
《中国食物与营养》
2017年第9期28-30,共3页
Food and Nutrition in China
关键词
二极管阵列高效液相色谱
三重四级杆液质联用
三聚氰胺
豆奶
Diode Array High Performance Liquid Chromatography （HPLC-DAD）
Triple Level 4 Pole Liquid Ms （LC/MS/MS）
melamine
soy milk
