摘要
采用分散固相萃取净化,亲水作用色谱串联质谱分离检测,建立了荸荠中高氯酸盐的检测方法。对荸荠中高氯酸盐的提取和净化条件进行了优化:提取溶剂为含1%乙酸的乙腈/水(V:V,1:1),提取时间2 min,净化材料为100 mg GCB和100 mg C18。在此条件下,高氯酸盐在1~50μg/L浓度范围内呈现良好的线性关系,相关系数(R^2)为0.9992,定量限为10μg/kg,在10,40,200μg/kg添加水平的回收率分别为101.6%,86.0%和110.2%,日内日间相对标准偏差低于12.3%,该方法具有很好的灵敏度、准确度和精密度。将所建立的方法用于41个荸荠样品中高氯酸盐的风险监测,取得了较好的效果。
A method for the determination of perchlorate in water chestnut by disperse solid phase extraction(dSPE)cleanup coupled with ultra-high performance liquid chromatography tandem mass spectrometry(UPLCMS/MS)was proposed.The extraction conditions were optimized:acetonitrile/water(V:V,1:1)with 1%acetic acid as extraction solvent,2 min of extraction time,100 mg graphitized carbon black(GCB)and 100 mg C18 as sorbents of dSPE.Under the optimized conditions,perchlorate showed a good linear relationship in the range of1-50μg/L with R^2 of 0.9992 and LOQ of 10μg/kg.The recoveries of perchlorate spiked at 10,40 and200μg/kg were 101.6%,86.0%and 110.2%,respectively.The inter-day and intra-day relative standard deviations were lower than 12.3%,demonstrating high accuracy and precision of the proposed method.Finally,the proposed method was applied for the risk monitoring of perchlorate in 41 water chestnut samples.
作者
张惠贤
郑丹
夏虹
夏珍珍
胡西洲
彭西甜
ZHANG Huixian;ZHENG Dan;XIA Hong;XIA Zhenzhen;HU Xizhou;PENG Xitian(Institute of Agricultural Quality Standards and Testing Technology Research,Hubei Academy of Agricultural Science/Laboratory of Quality&Safety Risk Assessment for Agro-products(Wuhan),Ministry of Agriculture and Rural Affairs,Wuhan 430064)
出处
《分析试验室》
CAS
CSCD
北大核心
2020年第8期899-903,共5页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金项目(21607039)
国家农产品质量安全风险评估项目(GJFP2019039)资助。
关键词
荸荠
高氯酸盐
分散固相萃取
亲水作用色谱-串联质谱
perchlorate
water chestnut
ultra-high performance liquid chromatography tandem mass spectrometry
