食品科学 ›› 2022, Vol. 43 ›› Issue (2): 310-315.doi: 10.7506/spkx1002-6630-20210425-351

• 安全检测 • 上一篇    下一篇

超高效液相色谱-三重四极杆质谱联用检测饮用水中N-亚硝胺类消毒副产物

孙铭,古其会,张菊梅,郭伟鹏,吴慧清,张友雄,韦献虎,吴清平   

  1. (1.中国科学院广州化学研究所,广东 广州 510650;2.广东省科学院微生物研究所,华南应用微生物国家重点实验室,广东省微生物安全与健康重点实验室,广东 广州 510070;3.中国科学院大学,北京 100049)
  • 出版日期:2022-01-25 发布日期:2022-01-29
  • 基金资助:
    国家自然科学基金青年科学基金项目(31901663);广东省科技计划项目(2020B121202009); 广东省科学院发展专项(2019GDASYL0103006)

Determination of N-Nitrosamine Disinfection By-products in Drinking Water by Ultra-high Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

SUN Ming, GU Qihui, ZHANG Jumei, GUO Weipeng, WU Huiqing, ZHANG Youxiong, WEI Xianhu, WU Qingping   

  1. (1. Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650, China;2. Guangdong Provincial Key Laboratory of Microbial Safety and Health, State Key Laboratory of Applied Microbiology Southern China, Institute of Microbiology, Guangdong Academy of Sciences, Guangzhou 510070, China;3. University of Chinese Academy of Sciences, Beijing 100049, China)
  • Online:2022-01-25 Published:2022-01-29

摘要: 为评估饮用水中新型消毒副产物N-亚硝胺对食品饮料行业带来的潜在风险,建立一种基于超高效液相色谱-三重四极杆质谱联用仪同时检测饮用水中9 种N-亚硝胺类消毒副产物的方法。样品通过固相萃取,进入超高效液相色谱-质谱检测系统,经RRHD-C18色谱柱分离,以含有0.2%甲酸的10 mmol/L碳酸氢铵溶液和甲醇作为流动相梯度洗脱,采用大气压化学电离正离子多反应监测扫描模式检测。在优化条件下9 种N-亚硝胺在一定质量浓度范围内线性关系良好,相关系数大于0.996,方法检出限为0.10~0.33 ng/L,方法的回收率为62.1%~118.2%,相对标准偏差为2.2%~10.0%,分析时间为6 min。与现有方法比较,本方法灵敏度高、检测速度快、适用性强,能满足食品饮料生产中饮用水N-亚硝胺类消毒副产物的检测需求。

关键词: 超高效液相色谱-三重四极杆质谱;N-亚硝胺类消毒副产物;固相萃取;饮用水

Abstract: In order to evaluate the potential risks posed by N-nitrosamines, a group of emerging disinfection by-products in drinking water, to the food and beverage industry, a method based on ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of nine N-nitrosamine disinfection by-products in drinking water. The samples were extracted by solid phase extraction. The chromatographic separation was accomplished on a RRHD-C18 column with gradient elution using a mobile phase consisting of 10 mmol/L ammonium bicarbonate aqueous solution containing 0.2% formic acid and methanol. The detection was carried out using an atmospheric pressure chemical ionization (APCI) source in a multi-reaction monitoring (MRM) mode. Under optimized conditions, the calibration curves for nine N-nitrosamines were linear in a certain concentration range, with correlation coefficient greater than 0.996, and the detection limit of the developed method was 0.10–0.33 ng/L. The spiked recoveries of the method were 62.1%–118.2%, with relative standard deviation (RSD) of 2.2%–10.0%. The analysis process took 6 min. Compared with the existing methods, this method is very sensitive, fast and highly applicable, and can meet the requirements for the detection of N-nitrosamine disinfection by-products in drinking water for food and beverage production.

Key words: ultra-high performance liquid chromatography-triple quadrupole mass spectrometry; N-nitrosamine disinfection by-products; solid phase extraction; drinking water

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