高效液相色谱-串联质谱法测定食品用纸制品中氯酚类化合物残留量
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(北京市丰台区疾病预防控制中心,北京 100071)

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张志荣 男 主管技师 研究方向为卫生理化检验 E-mail:zhangzhirongxxx@126.com通信作者:┣┣(中)通信作者┫┫信振江 男 副主任医师 研究方向为公共卫生 E-mail:xzjsnow@163.com

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Determination of chlorophenols in food paper products by high performance liquid chromatography-tandem mass spectrometry
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(Fengtai Center for Disease Control and Prevention, Beijing 100071, China)

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    摘要:

    目的 建立高效液相色谱-串联质谱(HPLC-MS/MS)同时测定食品用纸制品中2,4-二氯酚、2,4,6-三氯酚、2,3,4,6-四氯酚、五氯酚4种氯酚类化合物残留量的检测方法。方法 样品经0.5%甲酸甲醇超声提取后,混合型阴离子交换固相萃取柱净化,以HSS T3色谱柱(2.1 mm×100 mm,1.8 μm)分离待测物,采用电喷雾离子化,负离子扫描和多反应监测模式(MRM)检测,以保留时间和特征离子对定性,内标法定量。结果 4种待测物在5~100 μg/L浓度范围内线性关系良好,相关系数(r)均大于0.99;方法检出限为0.01~0.02 mg/kg,定量限为0.03~0.06 mg/kg;4种物质的添加水平为0.03~0.14 mg/kg时,平均回收率为80.1%~110.4%,相对标准偏差为3.2%~9.9%(n=6)。结论 该方法样品前处理简单,准确性、精密度和灵敏度均较好,适用于食品用纸制品中4种氯酚类化合物残留量的检测。

    Abstract:

    Objective To establish a method for simultaneous determination of the residues of four chlorophenols compounds (2,4-dichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) in food paper products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted by ultrasonic 0.5% formic acid in methanol and purified by mixed anion exchange solid phase column. The target compounds were separated on HSS T3 column(2.1 mm×100 mm,1.8 μm), and detected under negative ionization and multiple reaction monitoring(MRM) mode. Four compounds were identified by retention time and the ratio of characteristic ions, and were quantified by using the internal standard method. Results The calibration curves of the four compounds were linear within the range from 5 to 100 μg/L. The correlation coefficients of the four compounds were above 0.99.The limits of detection(LOD)were in the range of 0.01-0.02 mg/kg,and the limits of quantification(LOQ)were in the range of 0.03-0.06 mg/kg. The average recoveries of paper samples at spiked levels from 0.03 to 0.14 mg/kg were between 80.1% and 110.4%, and the relative standard deviations (n=6) were between 3.2% and 9.9%. Conclusion The pretreatment of sample was simple. The method was accurate and sensitive, which could be used to determine chlorophenols compounds in food paper products.

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张志荣,张来颖,王玉江,刘裕婷,信振江.高效液相色谱-串联质谱法测定食品用纸制品中氯酚类化合物残留量[J].中国食品卫生杂志,2019,31(3):226-230.

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  • 收稿日期:2019-04-25
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  • 在线发布日期: 2019-07-09
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