简龙海, 韩晶, 郑荣, 王柯. LC-APCI-MS/MS法检测食品中N-二甲基亚硝胺的方法[J]. 上海预防医学, 2019, 31(6): 427-431. DOI: 10.19428/j.cnki.sjpm.2019.19475
引用本文: 简龙海, 韩晶, 郑荣, 王柯. LC-APCI-MS/MS法检测食品中N-二甲基亚硝胺的方法[J]. 上海预防医学, 2019, 31(6): 427-431. DOI: 10.19428/j.cnki.sjpm.2019.19475
JIAN Long-hai, HAN Jing, ZHENG Rong, WANG Ke. Determination of N-dimethylnitrosamine in food by liquid chromatography-atmospheric chemical ionization-tandem mass spectrometry[J]. Shanghai Journal of Preventive Medicine, 2019, 31(6): 427-431. DOI: 10.19428/j.cnki.sjpm.2019.19475
Citation: JIAN Long-hai, HAN Jing, ZHENG Rong, WANG Ke. Determination of N-dimethylnitrosamine in food by liquid chromatography-atmospheric chemical ionization-tandem mass spectrometry[J]. Shanghai Journal of Preventive Medicine, 2019, 31(6): 427-431. DOI: 10.19428/j.cnki.sjpm.2019.19475

LC-APCI-MS/MS法检测食品中N-二甲基亚硝胺的方法

Determination of N-dimethylnitrosamine in food by liquid chromatography-atmospheric chemical ionization-tandem mass spectrometry

  • 摘要:
    目的建立水蒸气蒸馏,液相色谱-大气压化学离子化-串联质谱法(LC-APCI-MS/MS)测定食品中的N-二甲基亚硝胺(NDMA)的方法。
    方法样品加入同位素内标后,采用改进的水蒸气蒸馏法进行处理,馏出液用二氯甲烷萃取。萃取液加水1 mL后采用减压旋转蒸发仪浓缩(水浴温度为35℃,真空度为50 kPa)至无二氯甲烷。浓缩液用大气压化学离子化源-液相色谱-四极杆串联质谱仪测定。色谱柱为Poroshell 120 EC-C18柱(2.7 μm,4.6 mm×100 mm),流动相为甲醇-水系统。正离子多反应监测模式,内标法定量。
    结果在5~500 ng/mL范围内,N-二甲基亚硝胺的线性关系良好,加标回收率(添加水平分别为0.15、0.5、10 μg/kg)在80%~110%之间,相对标准偏差(RSD)小于7%,检出浓度为0.1 μg/kg。30批市售肉制品均未检出NDMA,30批市售熏烤鱼片、鱼干等水产制品中有19批检出NDMA,含量为0.38 μg/kg~15.7 μg/kg,其中2批样品的含量分别为8.45 μg/kg及15.7 μg/kg,超出国家标准中NDMA的限值规定(4.0μg/kg)。
    结论本方法灵敏度高,准确度好,适于食品中N-二甲基亚硝胺的测定。

     

    Abstract:
    ObjectiveTo establish a method for determination of N-dimethylnitrosamine in food by steam distillation-liquid chromatography-atmospheric chemical ionization-tandem mass spectrometry (LC-APCI-MS/MS).
    MethodsThe sample spiked with isotope internal standard was processed by improved steam distillation method, and the distillate extracted by dichloromethane.After adding 1 mL of water, the extract was concentrated to no dichloromethane by vacuum rotary evaporator (water bath temperature 35℃, vacuum 50 kPa).The concentrate was determined by LC-APCI-MS/MS.The residue was separated on a Poroshell 120 EC-C18 column (2.7 μm, 4.6 mm×100 mm) with the mobile of methanol-water system, then was monitored by positive multiple reaction monitoring (MRM) mode and quantified by internal Standard.
    ResultsThe calibration relations showed good linearity between 5 and 500 ng/mL.Recoveries at 0.15, 0.5 and 10 μg/kg were within 80%-110% with relative standard deviation (RSD) less than 7%.The detection concentration was 0.1 μg/kg.NDMA was not detected in 30 batches of meat products, but detected in 19 out of 30 batches of smoked and roasted fish fillets with content ranging from 0.38 μg/kg to 15.7 μg/kg.The content of NDMA in two batches of samples (8.45 μg/kg and 15.7 μg/kg, respectively) exceeded the limits of NDMA in Chinese GB 2762 (4.0 μg/kg).
    ConclusionThe method in this study is sensitive, accurate, and suitable for the determination of N-dimethylnitrosamine in food.

     

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