三重四级杆气相色谱-质谱法测定鸡肉中的五氯酚钠  

Determination of sodium pentachlorophenol in chicken by triple quadrupole gas chromatography-mass spectrometry

作　　者：秦玫[1] QIN Mei(Shizuishan Center for Disease Control and Prevention,Shizuishan,Ningxia 753000,China)

机构地区：[1]宁夏石嘴山市疾病预防控制中心

出　　处：《中国卫生检验杂志》2019年第17期2075-2077,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立三重四级杆气相色谱-质谱法测定鸡肉中五氯酚钠的含量,为国家食品污染和有害因素风险监测提供实验室依据,确保消费者食品安全。方法由于鸡肉样品基体对目标成分和内标物均具有抑制作用,以空白样品为基准加入2,4,6-三溴酚内标,经5%三氯乙酸沉淀,液液萃取,SLC柱净化,乙酸酐-吡啶溶液衍生,做工作曲线;选取最高响应的离子进行二次轰击,采用MRM法对测定结果进行定量,既能更为准确定量,又避免了因杂峰干扰带来的数据误差。结果以空白样品做工作曲线,浓度为2 ng/kg^40 ng/kg时,线性关系良好,相关系数为0.999 0,检出限为0.02μg/kg。在3种加标浓度下,加标回收率为98.1%~101.3%,相对标准偏差为0.647%~0.849%。结论本方法灵敏度高,适用于基质干扰较大的鸡肉样品。Objective To establish a triple quadrupole gas chromatography-mass spectrometry for the determination of sodium pentachlorophenol in chicken meat,so as to provide laboratory basis for national food contamination and risk monitoring of harmful factors to ensure food safety in consumers. Methods Because the chicken sample matrix had inhibitory effect on the target component and the internal standard,the internal standard of 2,4,6-tribromophenol was added with blank sample, precipitated by 5% trichloroacetic acid,liquid-liquid extraction,SLC column purification,acetic anhydride-pyridine solution derivation,and the work curve was made;The highest response ion was selected for secondary bombardment,MRM method was used to quantify the measurement results,which can not only accurately quantify,but also avoid the interference caused by the peak interference data error. Results The blank curve was used as the working curve. When the concentration ranged from 2 ng /kg to 40 ng /kg,the linear relationship was good,the correlation coefficient ( r) was 0. 999 0,and the detection limit was 0. 02 μg /kg. Under the three spiked concentrations,the recoveries were within 98. 1%-101. 3%,and the relative standard deviations were within 0. 647%-0. 849%. Conclusion This method has high sensitivity and is suitable for chicken samples with large matrix interference.

关 键 词：三重四级杆 气相色谱-质谱法 鸡肉 五氯酚钠 

分 类 号：O657.63[理学—分析化学]