摘要
目的建立高效液相色谱-串联质谱法测定茶叶中的高氯酸盐,并调查市售茶叶污染情况。方法采用稳定性同位素稀释技术,用0.2%乙酸提取,经石墨炭黑柱净化,以0.1%甲酸溶液-甲醇为流动相梯度洗脱,多反应监测模式(MRM)检测,内标法定量。结果高氯酸盐浓度在0.25~50.0μg/L范围内线性良好,加标回收率96%~102.1%,相对标准偏差0.9%~1.6%,定量限0.01mg/kg。茶叶中高氯酸盐检出率91.1%(112/123),含量均值196.5ng/g,中位值129.5ng/g(10.1~735ng/g)。茶叶中高氯酸盐检出率较高,按茶叶种类和生产地域比较含量差异不大。结论建立的方法具有操作简便、灵敏度高、稳定性好等优点,可较好地满足茶叶中高氯酸盐的检测需要。
Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS)method for detecting perchlorate in tea and investigate the contamination of commercial tea.Methods Using stable isotope dilution techniques,the sample was extracted with 0.2%acetic acid,cleaned with carboblack packed columns.The gradient elution was carried out with 0.1%formic acid solution as the mobile phase.Mass spectrometric detection was carried out by using multiple reaction monitoring mode(MRM)and quantified by internal standard.Results The calibration curves shown liner trend in the range of 0.35~50.0μg/L,the of recovery rates were from 96.0% to 102.1%,the relative standard deviation were from 0.9 to 1.6%,the detection limit were at 0.01 mg/kg level.The detection rate of the tea was 91.1%(112/123),the mean value was 196.5 ng/g,the median value was 129.5 ng/g(10.1-735 ng/g).The total detection rate of perchlorate in tea is relatively at the high level,with a little differences for the contents according to the comparison on tea types and production areas.Conclusion The method established showed the advantages with simple operation,high sensitivity and good stability,and can meet the needs of perchlorate detection in tea.
出处
《海峡预防医学杂志》
CAS
2018年第1期4-6,12,共4页
Strait Journal of Preventive Medicine
基金
福建省新型污染物生态毒理效应与控制重点实验室开放课题(No.PY16007)
关键词
茶叶
高氯酸盐
液相色谱-串联质谱法
污染
Tea
Perchlorate
Liquid Chromatography-Tandem Mass Spectrometry
Contamination
