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2~500ng/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0.1μg/kg,定量限为0.3μg/kg。在1、10、20和50μg/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。
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 coeffiicients greater than 0.995.In addition,the limit of detection was 0.1μg/kg the minimum detection value was 0.3μg/kg.At concentrations of 1,10,20 and 50μg/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.
作者
宋文龙
李一晗
SONG Wen-Long;LI Yi-Han(Shandong Xinjiaxiang Testing Technology Co.,Ltd.,Weifang 261000,China;College of Enology,Northwest Agriculture and Forestry University,Yangling 712100,China)
出处
《食品安全质量检测学报》
CAS
2024年第13期41-48,共8页
Journal of Food Safety and Quality
关键词
葡萄果实
高氯酸盐
超高效液相色谱-串联质谱法
grapes
perchlorate
ultra performance liquid chromatography-tandem mass spectrometry
