热水浴提取结合UPLC-MS/MS同时测定枸杞中氯酸盐和高氯酸盐  

Simultaneous determination of chlorate and perchlorate in wolfberry by hot water bath extraction combined with UPLC-MS/MS

作　　者：杨春霞 刘霞 王芳焕 牛艳 YANG Chunxia;LIU Xia;WANG Fanghuan;NIU Yan(Ningxia Quality Standards and Testing Technology Institute of Agricultural Product,Yinchuan 750002,China;Yinchuan Customs Technical Center,Yinchuan 750000,China)

机构地区：[1]宁夏农产品质量标准与检测技术研究所,宁夏银川750002 [2]银川海关技术中心,宁夏银川750000

出　　处：《中国酿造》2024年第2期258-263,共6页China Brewing

基　　金：宁夏回族自治区重点研发计划项目(2022BEG03069);2021年自治区人才专项青年拔尖人才项目;2022年自治区人才专项青年拔尖人才项目。

摘　　要：该研究建立了热水浴提取-分散固相萃取(DSPE)净化-超高效液相色谱-串联质谱(UPLC-MS/MS)测定枸杞干果、鲜果中氯酸盐和高氯酸盐含量的方法。试样用7 m L超纯水在60℃水浴中振荡提取30 min后,加入13 m L甲醇涡旋5 min,离心后上清液用C18和石墨化碳黑(GCB)组合分散固相萃取净化,净化液在电喷雾负离子源和多反应监测(MRM)模式下测定,基质外标法定量。结果表明,枸杞干果、鲜果中氯酸盐和高氯酸盐均分别在1.0~100.0 ng/mL、0.5~100.0 ng/mL范围内线性关系良好,相关系数R2分别为0.998 9和0.999 2及0.998 4和0.999 0。氯酸盐检出限(LOD)为1.0μg/kg、定量限(LOQ)为10.0μg/kg;高氯酸盐LOD为0.5μg/kg、LOQ为5.0μg/kg。干果中氯酸盐和高氯酸盐平均加标回收率分别为89.9%~93.4%和76.8%~93.6%,相对标准偏差(RSD)分别小于11.0%和12.0%;鲜果中氯酸盐和高氯酸盐平均加标回收率分别为73.8%~94.9%和61.2%~90.5%,RSD分别小于11.0%和17.0%。A method for the determination of chlorate and perchlorate in dried and fresh wolfberry by hot water bath extraction-dispersive solid phase extraction(DSPE)purification-ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The sample was extracted by 7 ml ultra-pure water with water bath oscillations at 60℃for 30 min,and then 13 ml methanol was added to vortex for 5 min.After centrifugation,the supernatants were purified by dispersed solid-phase extraction with C18 and graphitized carbon black(GCB).The purified liquid was determined under electrospray negative ion source and multiple reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that the linear relationship between chlorate and perchlorate in dried and fresh wolfberry was good within the range of 1.0-100.0 ng/ml and 0.5-100.0 ng/ml,respectively.The correlation coefficients R2 were 0.9989 and 0.9992,0.9984 and 0.9990,respectively.The limits of detection(LOD)and quantitation(LOQ)of chlorate were 1.0μg/kg and 10.0μg/kg,respectively,and the LOD and LOQ were 0.5μg/kg and 5.0μg/kg,respectively.The average adding standard recoveries of chlorate and perchlorate in dried and fresh wolfberry were 89.9%-93.4%and 76.8%-93.6%,respectively,with the relative standard deviations(RSD)lower than 11.0%and 12.0%,respectively.The average adding standard recoveries of chlorate and perchlorate were 73.8%-94.9%and 61.2%-90.5%,respectively,with RSD lower than 11.0%and 17.0%,respectively.

关 键 词：枸杞 氯酸盐 高氯酸盐 超高效液相色谱-串联质谱 热水浴提取 分散固相萃取净化 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]