摘要
建立了测定猪肉、牛肉中高氯酸盐的超高效液相色谱-串联质谱法。试样用甲醇-超纯水溶液(7︰3, V/V)提取,离心,上清液过PRiME HLB小柱净化,经色谱柱分离,多反应监测(MRM)负离子模式进行检测,外标法定量。高氯酸盐在0.05~5.00μg/L范围内呈现出良好的线性关系,相关系数为0.999 3,检出限为1μg/kg;在1, 2和10μg/kg三个添加水平下的回收率分别为:猪肉85.2%~98.8%和牛肉90.8%~106.0%;相对标准偏差(RSD)为猪肉1.97%~3.87%和牛肉1.14%~4.32%。该研究建立的方法操作简便、准确、重复性好、灵敏度高,能满足猪肉、牛肉中高氯酸盐的日常检测工作。
A method was developed for the determination of perchlorate in pork and beef by Ultra high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with methanol-ultrapure water solution(7︰3, V/V), and then centrifuged. The supernatant was purified by PRiME HLB column. The separation of perchlorate was carried out on chromatographic column, then the samples were detected by multi-reaction monitoring(MRM) anion mode, and quantified by external standard method. The linear relationship was good between 0.05 μg/L and 5.00 μg/L, correlation coefficients were more than 0.999 3, and the detection limit was 1 μg/kg. The results showed that the recoveries of perchlorate in pork and beef samples were 85.2%-98.8% and 90.8%-106.0%, respectively;And the relative standard deviations were 1.97%-3.87% and 1.14%-4.32%, respectively. The method was simple, accurate, reproducible and sensitive. It was suitable for daily determination of perchlorate in pork and beef and provided technical support for the detection and supervision of pork and beef products.
作者
黄永桥
马凯
吴新文
曹俊杰
简银池
HUANG Yongqiao;MA Kai;WU Xinwen;CAO Junjie;JIAN Yinchi(Guizhou Academy of Testing and Analysis,Guiyang 550000)
出处
《食品工业》
CAS
北大核心
2019年第12期298-300,共3页
The Food Industry
基金
贵州科学院青年基金（黔科院J合字[2017] 8号）
关键词
超高效液相色谱-串联质谱法
猪肉
牛肉
高氯酸盐
ultrahigh performance liquid chromatography-tandem mass spectrometry
pork
beef
perchlorate
