色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1064-1070.DOI: 10.3724/SP.J.1123.2019.04052

• 特别策划：固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

高效液相色谱-串联质谱法测定奶粉中氯酸盐和高氯酸盐

周晓晴1, 吕小丽1, 万建春1, 郭平1, 郭丹1, 席慧婷2   

  1. 1.江西省食品检验检测研究院, 江西 南昌 330001;
    2.南昌大学食品科学与技术国家重点实验室, 江西 南昌 330047
  • 收稿日期:2019-05-07 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 郭平,Tel:(0791)86258602,E-mail:765570276@qq.com.

Determination of chlorate and perchlorate in milk power by high-performance liquid chromatography-tandem mass spectrometry

ZHOU Xiaoqing1, LÜ Xiaoli1, WAN Jianchun1, GUO Ping1, GUO Dan1, XI Huiting2   

  1. 1. Jiang Xi Institute for Food Control, Nanchang 330001, China;
    2. State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China
  • Received:2019-05-07 Online:2019-10-08 Published:2020-12-11

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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，10000 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 μm），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 μg/L和1.0~20.0 μg/L范围内线性关系良好，相关系数（r2）大于0.999，方法的定量限分别为15.0和7.5 μg/kg。氯酸盐和高氯酸盐分别在30.0、60.0、120.0 μg/kg和15.0、30.0、60.0 μg/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。

关键词: 液相色谱-串联质谱法, 氯酸盐, 高氯酸盐, 奶粉

Abstract: 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 10000 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 μm) 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 μg/L, respectively, with correlation coefficients (r2) greater than 0.999. The limits of quantification (LOQs) of chlorate and perchlorate were found to be 15.0 and 7.5 μg/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 μg/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.

Key words: high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), chlorate, perchlorate, milk power

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