Citation: ZHOU Xiaoqing, LÜ Xiaoli, WAN Jianchun, GUO Ping, GUO Dan, XI Huiting. Determination of chlorate and perchlorate in milk power by high-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(10): 1064-1070. doi: 10.3724/SP.J.1123.2019.04052 shu

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

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 Date: 7 May 2019

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.
- high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- chlorate,
- perchlorate,
- milk power
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1.
沈阳化工大学材料科学与工程学院沈阳 110142