摘要
建立了一种测定奶粉中氯酸盐和高氯酸盐含量的高效液相色谱-串联质谱方法。样品经0.1%(v/v)甲酸水-乙腈提取, 10 000 r/min 下离心10 min后,上清液经PRiME HLB固相萃取柱净化;采用离子交换色谱分离,色谱柱为Thermo Scientific Acclaim TRINITY P1复合离子交换柱(50 mm×2.1 mm, 3 μ m),以乙腈和20 mmol/L 乙酸铵溶液为流动相进行梯度洗脱,MS/MS检测,内标法定量。结果显示,氯酸盐和高氯酸盐分别在2.0~40.0 μ g/L 和1.0~20.0 μ g/L 范围内线性关系良好,相关系数( r^2)大于0.999,方法的定量限分别为15.0和7.5 μ g/kg 。氯酸盐和高氯酸盐分别在30.0、60.0、120.0 μ g/kg 和15.0、30.0、60.0 μ g/kg 3个水平下的加标回收率为89.24%~107.85%,相对标准偏差为3.15%~10.42%( n =6)。该方法简便快捷、准确可靠,能适用于奶粉样品的测定。
An analytical method based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for detecting chlorate and perchlorate residues in milk power.Chlorate and perchlorate in milk power were extracted using a 0.1%(v/v) formic acid-acetonitrile solution.The extract was centrifuged at 10 000 r/min for 10 min, and the supernatant was cleaned up on a PRiME HLB column.Separation of chlorate and perchlorate was performed on an ion-exchange column (Thermo Scientific Acclaim TRINITY P1, 50 mm×2.1 mm, 3 μ m) by gradient elution using acetonitrile and 20 mmol/L ammonium acetate solution as the mobile phase.The analytes were identified by MS/MS.Quantification was achieved using internal standards.Chlorate and perchlorate demonstrated good linearity in the ranges of 2.0-40.0 and 1.0-20.0 μ g/L , respectively, with correlation coefficients ( r^2) greater than 0.999.The limits of quantification (LOQs) of chlorate and perchlorate were found to be 15.0 and 7.5 μ g/kg , respectively.The recoveries of chlorate and perchlorate ranged from 89.24% to 107.85% at the three spike levels of 30.0, 60.0, and 120.0, and 15.0, 30.0, and 60.0 μ g/kg , respectively, with relative standard deviations (RSDs) ranging from 3.15% to 10.42%( n =6).This method is convenient, rapid, accurate, and efficient, thus demonstrating its suitability for use in the determination of chlorate and perchlorate in milk power.
作者
周晓晴
吕小丽
万建春
郭平
郭丹
席慧婷
ZHOU Xiaoqing;L Xiaoli;WAN Jianchun;GUO Ping;GUO Dan;XI Huiting(Jiang Xi Institute for Food Control,Nanchang 330001,China;State Key Laboratory of Food Science and Technology,Nanchang University,Nanchang 330047,China)
出处
《色谱》
CAS
CSCD
北大核心
2019年第10期1064-1070,共7页
Chinese Journal of Chromatography
关键词
液相色谱-串联质谱法
氯酸盐
高氯酸盐
奶粉
high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
chlorate
perchlorate
milk power
作者简介
通讯联系人:郭平,Tel:(0791)86258602,E-mail:765570276@qq.com.
