超声提取土壤中苯酚的气相色谱-质谱检测方法研究  

Studies on the ultrasonic extraction and GC-MS determination of phenol in soil

作　　者：蒲彦利[1] 徐虹[1] 张春玲[1] 易承学[1] 曹文婷[1] PU Yan-li;XU Hong;ZHANG Chun-ling;YI Cheng-xue;CAO Wen-ting(Zhenjiang Municipal Center for Disease Control and Prevention, Jiangsu Zhenjiang 212004, China)

机构地区：[1]镇江市疾病预防控制中心,江苏镇江212004

出　　处：《江苏预防医学》2019年第2期138-140,223,共4页Jiangsu Journal of Preventive Medicine

基　　金：镇江市重点研发计划(社会发展)SH2018017

摘　　要：目的建立土壤中苯酚的气相色谱-质谱(GC-MS)快速检测方法。方法对土样提取方法和参数(包括溶剂、添加盐、超声时间、冷冻和干燥等)进行优化后,以HP-5MS毛细管色谱柱分离、质谱仪检测,以外标法定量。结果经优化样品以丙酮/正己烷(1:1)、添加1.0g NaCl及0.2g无水Na_2SO_4、超声20min提取土样中苯酚,土样可-40℃冷冻1周保存但不能冷冻干燥保存。苯酚在0.052 5～5.25μg/mL质量浓度范围内线性关系良好(r=0.997),检出限为0.005mg/kg,定量限为0.015mg/kg。低、中、高浓度加标回收率在84.3%～104.8%,RSD均<6.0%。结论建立的方法前处理简单、快速,准确度和精密度较高,可用于土壤中苯酚的日常快速确证及定量测定。Objective To establish a rapid determination assay of phenol in soil by gas chromatography-mass spectrometry(GC-MS).Methods The extraction methods and parameters(including solvent,salt,ultrasonic time,freezing and drying)of soil samples were optimized.The phenol in soil was extracted and separated by HP-5 MS capillary column.GC-MS detector was used to analyze the concentration,the external method was used for quantification.Results After optimization,the phenol in soil samples were extracted with acetone/n-hexane(1:1),with 1.0 g NaCl and 0.2 g anhydrous Na2SO4 and subjected to ultrasonic treatment for 20 min.The soil samples could be frozen at-40℃for 1 w,but could not be frozen-dried.Good linear relationship was obtained in concentration range of 0.052 5-5.25μg/mL for phenol(r=0.997).The limit of detection for phenol was 0.005 mg/kg,the limit of quantification was 0.015 mg/kg.The average recovery rates for spiked samples at low,medium and high concentration were 84.3%-104.8%,all relative standard deviations(RSDs)were less than 6%.Conclusion The established assay requires simple pre-treatment,it is quick with high accuracy and precision,which could be applied in routine quick confirmation and analysis for phenol in soil samples.

关 键 词：土壤 苯酚 超声 气相色谱-质谱联用法 

分 类 号：R113[医药卫生—公共卫生与预防医学]