摘要
目的建立液相色谱串联质谱检测饲料中高氯酸盐含量的方法。方法饲料样品经乙腈-水(2:1,V:V)超声提取,高速离心后,上清液经石墨炭黑固相萃取柱净化,液相色谱串联质谱测定,内标法定量。结果高氯酸盐在0~100ng/mL浓度范围内呈良好线性关系(r2=0.9998)。本方法的定量限为15.0μg/kg。高氯酸盐在15~150μg/kg添加浓度范围内,回收率为95.1%~102.4%,相对标准偏差为1.13%~9.82%。结论本方法前处理简单,具有较高准确度、灵敏度、稳定性,可以满足饲料中高氯酸盐的含量检测。
Objective To established a method for the determination of perchlorate content in forage by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Samples of forage were ultrasound extracted by acetonitrile-aqueous solution(2:1,V:V)and centrifugated at a high speed.Then the supernatant was purified by graphitized carbon black solid phase extraction column,and determined by LC-MS/MS,then quantified by internal standard method.Results The perchlorate showed a good linear relationship in the concentration range of 0–100 ng/mL(r2=0.9998).The quantitative limit of the method was 15.0μg/kg.The recoveries rate of perchlorate in the range of 15–150μg/kg was 95.1%-102.4%and relative standard deviations were 1.13%–9.82%.Conclusion This method has the advantages of simple pretreatment,high accuracy,sensitivity and stability,and can satisfy the determination of perchlorate content in feed.
作者
马晓冲
王瑶
李兴佳
柴艳兵
张耀广
李飞
MA Xiao-Chong;WANG Yao;LI Xing-Jia;CHAI Yan-Bing;ZHANG Yao-Guang;LI Fei(Junlebao Dairy Group,Shijiazhuang Key Laboratory of Dairy Quality and Safety Control,Ministry of Agriculture and Villages,Shijiazhuang 050021,China)
出处
《食品安全质量检测学报》
CAS
2020年第13期4171-4176,共6页
Journal of Food Safety and Quality
基金
“十三五”国家重点研发计划重点专项(2018YFC1604304)。
关键词
饲料
高氯酸盐
液质联用
同位素内标法
含量检测
forage
perchlorate
liquid chromatography-tandem mass spectrometry
isotopic internal standard method
content determination
