液相色谱-串联质谱法同时测定液体奶中的氯酸盐和高氯酸盐

Simultaneously determination of chlorate and perchlorate in liquid milk by liquid chromatography-tandem mass spectrometry

中文关键词:  液体奶  高氯酸盐  氯酸盐  液相色谱串联质谱法  回收率

英文关键词:liquid milk  perchlorate  chlorate  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时检测液体奶中氯酸盐和高氯酸盐的方法。方法 以液体奶为基质, 采用LC-MS/MS测定其中氯酸盐和高氯酸盐的污染水平, 对仪器条件, 试样的样本提取, 样本净化等进行测试优化, 并对优化的方法进行方法学考察。结果 优化后的检测方法采用ACQUITY UPLC?HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm), 流动相为乙腈和0.1%甲酸水溶液, 流速为0.1 mL/min, 进样量为5 μL。样品中提取液为2.0 mL 0.1%甲酸水溶液和8.0 mL乙腈, 固相萃取柱为SelectCore HLB-V高氯酸盐专用柱(150 mg/3 mL), 内标法定量检测液体奶中氯酸盐及高氯酸盐含量。经方法学考察氯酸盐和高氯酸盐在各自线性范围内线性关系良好, 氯酸盐与高氯酸盐溶剂标准曲线决定系数分别为0.9995、0.9998。氯酸盐检出限为2.4 μg/kg, 高氯酸盐检出限为0.8 μg/kg。实际样品检测加标回收率在81.9%~105.4%, 相对标准偏差小于10%, 满足定量检测需求。结论 该方法具有操作简便, 灵敏度高, 定量准确, 重复性好等特点, 适合基质较复杂的液体奶中氯酸盐和高氯酸盐的同时检测。

英文摘要:

      Objective To establish a method for the simultaneous deterction of chlorate and perchlorate in liquid milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Using liquid milk as the base, the contamination levels of chlorate and perchlorate were determined by LC-MS/MS. The instrument conditions, sample extraction and sample purification were tested and optimized, and the methodology of the optimized method was investigated. Results The optimized detection method employed an ACQUITY UPLC?HSS T3 chromatographic column (2.1 mm×100 mm, 1.8 μm), with the mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution, at a flow rate of 0.1 mL/min and an injection volume of 5 μL. The extract from the sample was 2.0 mL of 0.1% formic acid aqueous solution and 8.0 mL of acetonitrile. The solid-phase extraction column was used the SelectCore HLB-V high chlorate-specific column (150 mg/3 mL). The internal standard method was used for quantitative detection of chlorate and perchlorate in liquid milk. The linear relationship of chlorate and perchlorate in their respective linear ranges was good. The determination coefficient of chlorate was 0.9995, and that of perchloric acid salt was 0.9998. The limit of detection chlorate was 2.4 μg/kg and that of perchlorate was 0.8 μg/kg. The recovery rate of actual sample detection with spiked samples was between 81.9% and 105.4%. The relative standard deviation (RSD) was less than to 10%, meeting the requirements for quantitative detection. Conclusion This method has the characteristics of simple operation, high sensitivity, accurate quantification and good repeatability. It is suitable for the simultaneous detection of chlorate and perchlorate in complex liquid milk matrices.