高效液相色谱联用质谱法测定羊奶粉中的氯酸盐和高氯酸盐  

Determination of chlorate and perchlorate in goat milk powder by HPLC-MS/MS

作　　者：许小茜 李清清 顾颖娟 Xu Xiaoqian;Li Qingqing;Gu Yingjuan(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)

机构地区：[1]上海质量监督检验技术研究院,上海200233

出　　处：《分析仪器》2020年第5期46-51,共6页Analytical Instrumentation

基　　金：上海市市场监督管理局科研项目(2018-34)。

摘　　要：建立了高效液相色谱-串联质谱法测定羊奶粉中氯酸盐和高氯酸盐的残留量。样品经0.1%甲酸水溶解后,超声提取,乙腈除蛋白,10000r/min下离心10分钟后,上清液经PRiME HLB固相萃取柱净化。经Thermo Scientific Acclaim TRINITY P1色谱柱(50mmx2.1mm,3μm)分离,在流动相为浓度20mmol/L的甲酸铵水溶液和乙腈,流速0.4mL/min的条件下进行梯度洗脱,MS-MS检测,内标法定量。在该优化条件下,氯酸盐和高氯酸盐分别在2.0~100.0μg/L和1.0~50.0μg/L的范围内呈良好的线性(R^2≥0.999),定量限分别为15.0μg/kg和7.5μg/kg,氯酸盐方法回收率为95.7%~107.2%,相对标准偏差(RSD)为1.43%~3.66%;高氯酸盐方法回收率为96.1%~108.6%,相对标准偏差(RSD)为2.46%~4.04%。经测定多种市售羊奶粉,表明该方法操作简单、测定结果准确,可用于羊奶粉中氯酸盐和高氯酸盐残留的同时快速测定。After being dissolved in 0.1%(v/v)formic acid-acetonitrile solution,the sample of goat milk power was extracted by ultrasonic wave,deproteinized by acetonitrile,centrifuged at 10000r/min for 10 min.The supernatant was purified on a PRiME HLB column.Chlorate and perchlorate were separated with a Thermo Scientific Acclaim TRINITY P1 column at the flow rate of 0.4 mL/min by gradient elution,using acetonitrile and 20 mmol/L ammonium formate as mobile phase.The analytes were identified by MS/MS,and quantification was achieved using internal standards.Chlorate and perchlorate demonstrated good linearity in the range of 2.0-100.0μg/L and 1.0-50.0μg/L,respectively,with good linearity(R^2≥0.999).The limits of quantification(LOQs)of chlorate and perchlorate were 15.0μg/kg and 7.5μg/kg,respectively.The recoveries of chlorate and perchlorate ranged from 95.7%to 108.6%,respectively,with relative standard deviations(RSDs)ranging from 1.43%to 4.04%(n=7).This method is convenient,rapid,accurate,and efficient.

关 键 词：液质联用仪 氯酸盐 高氯酸盐 羊奶粉 

分 类 号：O657.63[理学—分析化学] TS252.51[理学—化学]