摘要
目的建立超高效液相色谱-四极杆静电场轨道阱高分辨质谱法快速检测液态奶中的氯酸盐和高氯酸盐的分析方法。方法样品经乙腈提取后,–20℃冷冻30 min,取上清液直接上机测定。在流速0.5 mL/min下,以乙腈-0.1%氨水溶液作为流动相,梯度洗脱分离。采用平行反应监测模式扫描,同位素内标法进行定量。结果氯酸盐、高氯酸盐分别在0.4~200.0、0.2~100.0 ng/mL范围内线性关系良好,相关系数均大于0.995。氯酸盐检出限为0.20μg/kg、高氯酸盐检出限为0.11μg/kg。样品加标回收率为86.8%~105.4%,日内精密度为4.2%~9.6%,日间精密度为3.5%~9.8%。应用建立的方法对185份液态奶进行测定,氯酸盐检出率为7.0%,浓度为2.12~8.14μg/kg,高氯酸盐检出率为82.2%,浓度为1.28~11.25μg/kg。检测结果与采用2020年国家食品污染物和有害因素风险监测工作手册食品中氯酸盐和高氯酸盐检测方法检测结果一致。结论该方法操作简便、快速、准确性高,适用于液态奶中氯酸盐、高氯酸盐的定性和定量分析。
Objective To establish a method for rapid determination of chlorate and perchlorate in liquid milk by ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry.Methods After extraction with acetonitrile,the samples were frozen for 30 min at–20℃,and the supernatant was taken directly to the machine for determination.At the flow rate of 0.5 mL/min,acetonitrile-0.1%ammonia solution was used as mobile phase,and gradient elution was performed.Parallel reaction monitoring mode scanning and isotope internal standard method were used for quantification.Results The linear range of chlorate and perchlorate were 0.4–200.0 and 0.2–100.0 ng/mL,respectively,with the correlation coefficients both greater than 0.995.The limits of detection were 0.20μg/kg for chlorate and 0.11μg/kg for perchlorate,respectively.The recoveries were 86.8%–105.4%,the intraday precision were 4.2%–9.6%,and the inter-day precision were 3.5%–9.8%.The method was applied to the determination of 185 liquid milk samples,the detection rates of chlorate and perchlorate were 7.0%and 82.2%,respectively,with concentration ranges 2.12–8.14μg/kg and 1.28–11.25μg/kg,respectively.The results were consistent with the detection results of chlorate and perchlorate in food by using the method for determination of chlorate and perchlorate in food from National Work Manual on Risk Monitoring of Food Contaminants and Harmful Factors 2020.Conclusion This method is simple,rapid and accurate,and suitable for the qualitative and quantitative analysis of chlorate and perchlorate in liquid milk.
作者
林强
杨超
李美丽
王佳
侯瀚然
邵兵
牛宇敏
LIN Qiang;YANG Chao;LI Mei-Li;WANG Jia;HOU Han-Ran;SHAO Bing;NIU Yu-Min(Beijing Yanqing District Center for Disease Prevention and Control,Beijing 102100,China;Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第10期3259-3265,共7页
Journal of Food Safety and Quality
基金
北京市食品风险监测项目(BJSP2021101245)
2022年首都卫生发展科研专项(2022-2G-3016)。
关键词
氯酸盐
高氯酸盐
液态奶
冷冻诱导液液萃取
超高效液相色谱-四极杆静电场轨道阱高分辨质谱法
chlorate
perchlorate
liquid milk
freeze induced liquid-liquid extraction
ultra performance liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry
