液相色谱串联质谱法测定调味品中氯酸盐和高氯酸盐
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(1.北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京 100013;2.北京市预防医学研究中心, 北京 100013;3.中国医科大学公共卫生学院,辽宁 沈阳 110013)

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孟娟 女 主管技师 研究方向为色谱分析E-mail:mengj777@sina.com

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国家自然科学基金重点项目(U1736201);国家重点研发计划(2017YFE0110800)


Determination of chlorate and perchlorate in seasoning by ultra performance liquid chromatography-tandem mass spectrometry
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(1.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China;2.Beijing Center for Preventive Medicine Research, Beijing 100013, China;3.School of Public Health, China Medical University, Liaoning Shenyang 110013, China)

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    摘要:

    目的 建立调味品中氯酸盐和高氯酸盐的超高效液相色谱三重四极杆质谱(ultra-performance liquid chromatography tandems mass spectrometry,UPLC-MS/MS)测定方法,对市售调味品样品进行检测。方法 调味品用水和酸化的乙腈溶液超声提取,提取液经石墨化炭黑柱(GCB)和Ag/H固相萃取小柱净化,采用UPLC-MS/MS 多反应监测模式测定,同位素内标校正曲线法定量。结果 氯酸盐和高氯酸盐的线性范围分别为1~1 000 μg/L和0.10~100 μg/L,相关系数 R2≥0.99。调味品中氯酸盐的检出限为3.0 μg/kg,定量限为10.0 μg/kg;高氯酸盐的检出限为0.3 μg/kg,定量限为1.0 μg/kg。两种目标化合物在三个加标水平下的平均回收率为 86.5%~113.7%,相对标准偏差RSD为1.8%~15.3%。122件调味品中氯酸盐和高氯酸盐的检出率分别是76.2%(93/122)和93.4%(114/122),最高检出浓度分别为30.4 mg/kg和12.3 mg/kg。结论 本方法灵敏度高,重现性好,适用于调味品中的氯酸盐和高氯酸盐残留的测定;调味品中高氯酸盐的污染较为普遍,应进一步加强研究。

    Abstract:

    Objective To establish a method for the determination of chlorate and perchlorate in seasoning samples by ultra-performance liquid chromatography tandems mass spectrometry (UPLC-MS/MS). Methods Seasoning sample was ultrasonically extracted with acidic acetonitrile solution, and then purified with a graphitized carbon black (GCB) cartridge and an Ag/H cartridge. UPLC-MS/MS analysis was conducted under multi-reaction monitoring mode with isotope-labelled internal standard calibration for quantification. Results Chlorate and perchlorate showed a good linearity (R2≥0.99) in the range of 1-1 000 μg/L and 0.1-100 μg/L, respectively. The limits of detection for chlorate and perchlorate were 3.0 μg/kg and 0.3 μg/kg, as well as the limits of quantification were 10 μg/kg and 1.0 μg/kg, respectively. The average recoveries of two compounds in seasoning samples at three spiked levels were 86.5%-113.7% and the relative standard deviations were 1.8%-15.3%. The detection rates of chlorate and perchlorate from 122 seasoning samples were 76.2% and 93.4%, with the maximum concentration of 30.4 mg/kg and 12.3 mg/kg, respectively. Conclusion The method is suitable for qualitative and quantitative analysis of chlorate and perchlorate in seasoning. Further study should be focused on the perchlorate in seasoning products since its relative prevalence contamination.

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孟娟,陈容,范赛,张晶,邵兵.液相色谱串联质谱法测定调味品中氯酸盐和高氯酸盐[J].中国食品卫生杂志,2021,33(6):797-802.

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  • 收稿日期:2021-10-08
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  • 在线发布日期: 2022-01-04
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