固相萃取-气相色谱-串联质谱法测定木耳中五氯苯酚  

Determination of pentachlorophenol in agaric by solid phase extraction coupled with gas chromatography-tandem mass spectrometry

作　　者：卢忠魁 刘超 李鲤 李天娇 吕红英 李百洋 李凤林 LU Zhong-Kui;LIU Chao;LI Li;LI Tian-Jiao;LV Hong-Ying;LI Bai-Yang;LI Feng-Lin(College of Food Engineering,Jilin Agricultural Science and Technology University,Jilin 132101,China;Jilin Province Brewing Technology Innovation Center,Jilin 132101,China;Jilin Province Grain Deep Processing School Enterprise Joint Technology Innovation Laboratory,Jilin 132101,China)

机构地区：[1]吉林农业科技学院食品工程学院,吉林132101 [2]吉林省酿造技术科技创新中心,吉林132101 [3]吉林省谷物精深加工校企联合技术创新实验室,吉林132101

出　　处：《食品安全质量检测学报》2023年第22期233-240,共8页Journal of Food Safety and Quality

基　　金：吉林农业科技学院人才启动基金项目(20215010);吉林农业科技学院营养与健康食品科技团队项目(2019);国家重点研发计划项目(2021YFD1600903)。

摘　　要：目的建立固相萃取-气相色谱-串联质谱法(gaschromatography-tandemmassspectrometry,GC-MS/MS)测定木耳中五氯苯酚的分析方法。方法 以2,4,6-三溴苯酚为内标物,样品经5%三氯乙酸水溶液浸提,以乙酸乙酯/正己烷液-液分配法萃取五氯苯酚,经SLC(氧化铝/SCX)固相萃取柱净化样品提取液,乙酸酐衍生,HP-5MS毛细管柱(30m×0.25mm,0.25μm)分离样品,在多反应监测(multiplereactionmonitoring,MRM)模式下,采用内标法定量。结果 方法在五氯苯酚质量浓度1~100 ng/mL范围具有良好线性关系,线性相关系数大于0.9999,在方法线性范围内低、中、高3个浓度水平加标回收率在89.3%~108.7%之间,相对标准偏差2.1%~9.0%。方法检出限为0.06μg/kg,定量限为0.20μg/kg。结论 本方法灵敏度高,方法稳定,重现性好,可用于木耳样品中五氯苯酚的定性定量测定。Objective To establish an analytical methods for the pentachlorophenol in agaric by solid-extraction coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods Using 2,4,6-tribromophenol as the internal standard,the agaric samples were extracted with 5%trichloroacetic acid aqueous solution,and pentachlorophenol was extracted using ethyl acetate/n-hexane liquid-liquid extraction method.The samples extracted liquid were purified using SLC(alumina/SCX)solid-phase extraction column,followed by acetic anhydride derivatization and separated by HP-5MS capillary column(30 m×0.25 mm,0.25μm),and detected in multiple reaction monitoring(MRM)mode and quantitated using an internal standards method.Results The method had a good linear relationship in the range of mass concentration of pentachlorophenol from 1 to 100 ng/mL,and the linear correlation coefficient was greater than 0.9999,the recoveries of the pentachlorophenol at the 3 spiked concentrations were 89.3%‒108.7%and the relative standard deviations were 2.1%‒9.0%.The limit of detection was 0.06μg/kg,and the limit of quantitation was 0.20μg/kg.Conclusion This method has high sensitivity,stability and good reproducibility,and can be used for qualitative and quantitative determination of pentachlorophenol in agaric samples.

关 键 词：气相色谱-串联质谱法 五氯苯酚 木耳 

分 类 号：O657.63[理学—分析化学] TS219[理学—化学]