气相色谱串联质谱法检测木砧板中五氯苯酚  

Determination of pentachlorophenol in wooden chopping boards with gas chromatography-tandem mass spectrometry

作　　者：赵玉文 李泽冉 薛香菊 杨萌 吉文亮[2] 荣维广[2] ZHAO Yuwen;LI Zeran;XUE Xiangju;YANG Meng;JI Wenliang;RONG Weiguang(Department of Foods,Shandong Drug and Food Vocational College,Weihai,Shandong 264210,China;Institute of Physical and Chemical Detection,Jiangsu Provincial Center for Disease Control and Prevention,Nanjing,Jiangsu 210009,China)

机构地区：[1]山东药品食品职业学院食品系,山东威海264210 [2]江苏省疾病预防控制中心理化检验所,江苏南京210009

出　　处：《预防医学》2023年第9期825-828,共4页CHINA PREVENTIVE MEDICINE JOURNAL

基　　金：江苏省医学重点学科(实验室)流行病学项目(ZDX⁃KA2016008)。

摘　　要：目的通过微型化样品前处理过程,优化木砧板中五氯苯酚的检测方法。方法处理好的木砧板样品经8 mL丙酮+2 mL水超声提取30 min,5 mL提取溶液中加入1 mL的0.5 mol/L碳酸钾溶液,采用0.3 mL乙酸酐衍生,正己烷萃取,DB-5ms色谱柱(30 m×0.25 mm,0.25μm)分离,采用串联质谱法多反应监测模式检测,内标法定量。结果在0.01~0.2μg/mL范围内,线性良好,线性相关系数R2>0.999,方法的检出限为0.003 mg/kg,定量限为0.01 mg/kg。在0.003、0.01、0.03 mg/kg的加标浓度下,目标物的平均回收率为84.2%~96.7%,相对标准偏差为2.2%~6.1%。结论本方法操作简单、环保,准确度和灵敏度高,适用于木砧板中五氯苯酚的检测。Objective To optimize the determination of pentachlorophenol in wooden chopping boards through pretreat⁃ment of miniaturized samples.Methods The pretreated wooden chopping board samples were subjected to ultrasound extraction(1 mL of 0.5 mol/L K2CO3 added in 5 mL extraction solution)in 8 mL acetone and 2 mL water,followed by derivatization with 0.3 mL acetic anhydride,extraction with n-hexane and separation with DB-5ms column(30 m×0.25 mm,0.25μm).Gas chromatography tandem mass spectrometry(GC-MS/MS)was performed in multiple reaction monitoring(MRM)mode with quantitative analysis using the internal standard method.Results The GC-MS/MS assay showed a good linear relationship within the range of 0.01 to 0.2μg/mL(R2>0.999),with a 0.003 mg/kg limit of detec⁃tion and 0.01 mg/kg limit of quantitation.The mean recovery rates were 84.2%to 96.7%at spiked concentrations of 0.003,0.01 and 0.03 mg/kg,with relative standard deviation of 2.2%to 6.1%.Conclusions The established GC-MS/MS assay is easy to perform,environment-friendly,highly accurate and sensitivity,which is feasible for determination of pentachlorophenol in wooden chopping boards.

关 键 词：木砧板 五氯苯酚 气相色谱-串联质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]