气相色谱法测定竹木砧板及筷子中五氯酚钠  

Determination of sodium pentachlorophenate in bamboo cutting boards and chopsticks by gas chromatography

作　　者：董四平[1] 许琼[1] DONG Si-ping;XU Qiong(Jingzhou Municipal Center for Disease Control and Prevention,Jingzhou,Hubei 434000,China)

机构地区：[1]湖北省荆州市疾病预防控制中心,湖北荆州434000

出　　处：《中国卫生检验杂志》2022年第7期809-810,814,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的通过气相色谱-电子捕获检测器法(GC-ECD),建立一种适用于竹木砧板及筷子中五氯酚钠的快速检测方法,以期为竹木砧板及筷子中五氯酚钠残留量的分析提供参考。方法样品经粉碎后于离心管中,分别加水、三氯乙酸、提取液在60℃进行超声及提取。提取液经SLC净化,采用乙腈洗脱后氮吹至1.0 ml左右,加衍生试剂于60℃水浴反应15 min,加1 ml正己烷,取上层有机相测定。采用HP-5(30 m×0.32 mm,0.25μm)毛细管色谱柱分离,GC-ECD检测,保留时间定性,外标法定量。结果该方法在50μg/L~1000μg/L浓度内呈良好的线性关系(r=0.9993);方法检出限为0.014 mg/kg,定量限为0.05 mg/kg;加标浓度为50μg/kg和200μg/kg时,平均加标回收率分别为91.6%和98.4%,相对标准偏差(RSD)分别为0.91%和4.8%(n=6)。结论本方法检测仪器简单,灵敏度高、准确度好,分析时间短,适用于竹木砧板及筷子中五氯酚钠的测定。Objective Through gas chromatography-electron capture detector method(GC-ECD),a rapid detection method for sodium pentachlorophenol in bamboo cutting boards and chopsticks was established to analyze the residual amount of sodium pentachlorophenol in bamboo cutting boards and chopsticks for reference.Methods After the sample is pulverized,it is placed in a centrifuge tube.Water,trichloroacetic acid and the extraction solution are added separately at 60℃for ultrasonic extraction.The extract was purified by SLC,eluted with acetonitrile,and then blown with nitrogen to about 1.0 ml.Derivatization reagent was added to react in a water bath at 60℃for 15 min.1 ml ofn-hexane was added and the upper organic phase was taken for determination.The HP-5(30 m×0.32 mm,0.25μm)capillary column was used for separation,GC-ECD detection,retention time qualification,and external standard method for quantification.Results The method showed a good linear relationship within the concentration of 50μg/L-1000μg/L(r=0.9993);the detection limit of the method was 0.014 mg/kg,the limit of quantification was 0.05 mg/kg.When the spiked concentration was 50μg/kg and 200μg/kg,the average recovery rate of standard addition was 91.6%and 98.4%,and the relative standard deviation(RSD)was 0.91%and4.8%(n=6).Conclusion This method has simple detection equipment,high sensitivity,good accuracy,and short analysis time.It is suitable for the determination of sodium pentachlorophenol in bamboo cutting boards and chopsticks.

关 键 词：气相色谱 五氯酚钠 竹木砧板及筷子 

分 类 号：O657.71[理学—分析化学]