超高效液相色谱-串联质谱法测定葡萄果实中的高氯酸盐

Determination of perchlorate in grapes by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  葡萄果实  高氯酸盐  液相色谱质谱  检测

英文关键词:grapes  perchlorate  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法定量检测葡萄果实中高氯酸盐含量的分析方法。方法 以葡萄为基质, 测定了其中高氯酸盐的含量。前处理最终选择WAX固相萃取柱作为净化柱; 分析过程使用Hypercarb色谱柱, 柱温为40℃; 流动相采用甲醇-0.2%甲酸水体系, 流速为0.3 mL/min; 离子源采用电喷雾源负离子模式, 并通过多反应监测模式来测定葡萄果实中高氯酸盐含量。结果 经过试验发现当高氯酸盐的质量浓度处于2~500 ng/mL范围内, 浓度与对应的峰面积有着优秀的线性, 相关系数大于0.995。此外, 检出限为0.1 μg/kg, 定量限为0.3 μg/kg。在1、10、20和50 μg/kg的加标浓度水平下, 高氯酸盐回收率为80.6%~96.8%, 相对标准偏差为7.6%~8.5%。结论 用该方法进行预处理更加方便、快速, 且检测灵敏度高, 可满足葡萄果实中高氯酸盐测定要求。

英文摘要:

      Objective To establish a method for the determination of perchlorate in grapes by ultra performance liquid chromatography-tandem mass spectrometry. Methods The content of perchlorate was measured using grapes as the substrate; the pre-treatment ultimately selected WAX solid-phase extraction column as the purification column; the analysis process used a Hypercarb chromatography column at 40℃; the mobile phase used a methanol 0.2% formic acid water system, with a flow rate of 0.3 mL/min; the ion source used negative ion mode of electrospray source, and the content of perchlorate in grapefruits was determined through multiple reaction monitoring mode. Results It was found that when the concentration of perchlorate is within the range of 2–500 ng/mL, there was an excellent linearity between the concentration and the corresponding peak area, and the correlation coefficients greater than 0.995. In addition, the limit of detection was 0.1 μg/kg the minimum detection value was 0.3 μg/kg. At concentrations of 1, 10, 20 and 50 μg/kg, the recovery rates of perchlorate ranged from 80.6%–96.8%, with relative standard deviations ranged from 7.6%–8.5%. Conclusion The developed methods for preprocessing are more convenient, rapid, and has high detection sensitivity, which can meet the requirements for the determination perchlorate in grape fruits.