• 安全检测 •

### 基于Captiva EMR-Lipid净化的婴儿配方乳粉中氯酸盐和高氯酸盐的离子色谱-串联质谱测定

1. （1.江苏省疾病预防控制中心，江苏 南京 210009；2.拉萨市疾病预防控制中心，西藏 拉萨 850000）
• 出版日期:2021-06-25 发布日期:2021-06-29
• 基金资助:
江苏省青年医学人才项目（QNRC2016543）

### Determination of Chlorate and Perchlorate in Infant Formula Powder by Ion Chromatography Coupled with Tandem Mass Spectrometry Based on Captiva EMR-Lipid Clean-up

ZHANG Hao, JIANG Xiaohong, HUO Zongli

1. (1. Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China; 2. Lhasa Center for Disease Control and Prevention, Lhasa 850000, China)
• Online:2021-06-25 Published:2021-06-29

Abstract: The aim of this study was to develop a method for the determination of chlorate and perchlorate in infant formula powder by using non-suppressed ion chromatography-tandem mass spectrometry. After being dissolved in pure water, proteins in the samples were precipitated with acetonitrile. After centrifugation, the supernatant was cleaned up by using Captiva EMR-Lipid, which could remove lipids from the matrix. The resulting filtrate was analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). An aqueous solution containing 0.7 mol/L methylamine and acetonitrile were applied as the mobile phase. The separation was performed on an IonPac AS16 column. Data were collected by multi-reaction monitoring (MRM) in electrospray negative ionization mode. The quantitative analysis was carried out by the internal standard method. The calibration curves for chlorate and perchlorate showed a good linearity in the range of 5–200 and 1.25–50 μg/L with a correlation coefficient greater than 0.999, respectively. The recoveries of chlorate and perchlorate in positive samples at three different spiked levels were in a range of 98.8%–101% and 97.2%–112% with relative standard deviations (RSD) of 1.1%–2.6% and 1.3%–6.8%, respectively. The limits of detection (LOD) and limits of quantification (LOQ) of this method were 4.8 and 16 μg/kg for chlorate, and 1.6 and 5.0 μg/kg for perchlorate respectively. This method is suitable for the routine detection of chlorate and perchlorate in infant formula powder with the advantages of simple pretreatment and high accuracy.