糖诱导相分离/超高效液相色谱-高分辨质谱法测定牛奶中高氯酸盐含量

Determination of perchlorate content in milk by sugar-induced phase separation and ultra performance liquid chromatography-high resolution mass spectrometry

中文关键词:  高氯酸盐  糖析诱导  超高效液相色谱-高分辨质谱  牛奶  样品前处理

英文关键词:Perchlorate  Sugar induction  Ultra-high performance liquid chromatography-high resolution mass spectrometry  Milk  Sample preparation

中文摘要:

      目的 基于糖诱导相分离技术结合超高效液相色谱-高分辨质谱法（UHPLC-HRMS）,建立一种同步净化牛奶基质和富集高氯酸盐的样品前处理和含量测定方法。方法 样品制备采用乙腈为提取溶剂,木糖为相分离诱导剂。分析物经Poroshell 120(50 mm × 2.1 mm,1.9 μm)色谱柱分离分析，以甲醇-1%乙酸水溶液为流动相进行梯度洗脱。采用电喷雾负离子模式与单一离子监测((targeted single ion monitoring, tSIM)扫描模式结合同位素内标法定量。 结果 在0.1~20 μg/L的范围内,高氯酸盐线性关系良好((r2=0.9988)。方法检出限(limit of detection, LOD)和定量限(limit of quantification, LOQ)LOD和LOQ分别为0.1 μg/L和0.3 μg/L；3个加标水平下，回收率为88.7%~116.8%，RSD相对标准偏差为2.3%~8.1%。在30份牛奶样品的检测分析中,高氯酸盐的检出率达100%。结论 该方法操作简便,对样品净化效果良好,具有低成本、高灵敏度的优点,适用于牛奶中高氯酸盐检测。

英文摘要:

      Objective To establish a sample preparation and detection method for simultaneous purification of milk matrix and enrichment of perchlorate based on sugar-induced phase separation technique combined with ultra performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Methods Acetonitrile was used as extraction solvent and xylose was used as phase separation inducer for sample preparation. The analyte was separated using a Poroshell 120 (50 mm × 2.1 mm, 1.9 μ m) chromatographic column and eluted with a gradient using a methanol-1% acetic acid aqueous solution as the mobile phase. Quantification was performed by isotope internal standard method under electrospray negative ion mode and target single ion monitoring (targeted single ion monitoring, tSIM) acquisition mode. Results Perchlorate showed a good linearity (r2=0.9988) in the range of 0.1-20.0 μg/L. Method limit of detection (LOD) and limit of quantification (LOQ) were 0.1 μg/L and 0.3 μg/L, respectively. Recoveries ranged from 88.7% to 116.8% at the 3 spiked levels, with relative standard deviations ranging from 2.3% to 8.1%. Perchlorate was detected in 100% of the 30 milk samples. Conclusion The method is easy to operate, has a good effect on sample purification, and has the advantages of low cost and high sensitivity, which is suitable for the detection of perchlorate in milk.