摘要
[目的]建立亲水交互作用/高效液相色谱-串联质谱法(LC-MS/MS)测定茶叶中高氯酸盐的方法。[方法]采用水溶液萃取茶叶中高氯酸盐,经Oasis PRiME HLB固相萃取柱净化,用Obelisc R色谱柱分离,以高效液相色谱-串联质谱法测定,同位素内标法定量。[结果]Obelisc R色谱柱能良好地增加保留时间至4.9 min,高氯酸根在1~200 ng/mL线性良好(R^(2)>0.9996),回收率为79.3%~115.3%,相对标准偏差(RSD)≤9.4%,定量限为35μg/kg。[结论]该方法操作简单、分离效果好、灵敏度能满足欧盟拟定限量的要求,适用于茶叶中高氯酸盐残留测定,为我国进一步规范茶叶安全标准提供技术支持。
[Objective]To establish a high performance liquid chromatography with tandem mass spectrometry(LC-MS/MS)method for the determination of perchlorate in tea.[Method]Perchlorate in tea was extracted by aqueous solution and purified by Oasis PRiME HLB solid phase extraction column,separated by Obelisc R chromatographic column,determined by high performance liquid chromatography with tandem mass spectrometry,and quantified by isotope internal standard method.[Result]The retention time of Obelisc R column could be well increased to 4.9 minutes.The linearity of perchlorate was good at 1-200 ng/mL(R^(2)>0.9996),the recovery rate was 79.3%-115.3%,the relative standard deviation(RSD)was not greater than 9.4%,and the quantitative limit was 35μg/kg.[Conclusion]The method has the advantages of simple operation and good separation effect,of which the sensitivity meet the requirements of the limit formulated by the European Union.It is suitable for the determination of perchlorate residue in tea and can provide a reference and theoretical basis for further standardizing tea safety standards.
作者
何国成
叶少媚
何思聪
张益文
贾晓菲
HE Guo-cheng;YE Shao-mei;HE Si-cong(Zhongshan Quality Safety&Inspection Institute of Agricultural Products,Zhongshan,Guangdong 528437)
出处
《安徽农业科学》
CAS
2022年第12期171-173,共3页
Journal of Anhui Agricultural Sciences
基金
中山市社会公益科技研究项目(2019B2059)。
关键词
亲水交互作用
高效液相色谱-串联质谱法
高氯酸盐
保留时间
茶叶
Hydrophilic interaction
High performance liquid chromatography with tandem mass spectrometry(LC-MS/MS)method
Perchlorate
Retention time
Tea
