高效液相色谱-串联质谱法测定奶粉中氯酸盐和高氯酸盐

引用本文: 周晓晴, 吕小丽, 万建春, 郭平, 郭丹, 席慧婷. 高效液相色谱-串联质谱法测定奶粉中氯酸盐和高氯酸盐[J]. 色谱, 2019, 37(10): 1064-1070. doi: 10.3724/SP.J.1123.2019.04052 shu

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

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.
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

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:

English

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: 07 May 2019

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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沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱-串联质谱法测定奶粉中氯酸盐和高氯酸盐

English

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

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中国化学会秘书处

高效液相色谱-串联质谱法测定奶粉中氯酸盐和高氯酸盐

English

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

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