衍生化-液液萃取气相色谱法测定环境水体中苦味酸  

Determination of picric acid in environmental water by derivatization and liquid-liquid extraction gas chromatography

作　　者：冯玲玲[1] 林庆文[1] 李胜生[1] 陈园园[1] FENG Lingling;LIN Qingwen;LI Shengsheng;CHEN Yuanyuan(Institute of Geological Experiment of Anhui Province,Hefei 230001,China)

机构地区：[1]安徽省地质实验研究所,安徽合肥230001

出　　处：《化学分析计量》2023年第4期44-47,共4页Chemical Analysis And Meterage

摘　　要：建立衍生化-液液萃取气相色谱法测定环境水体中的苦味酸。环境水体中的苦味酸经次氯酸钠氯化衍生后,用正己烷提取后进行气相色谱分析。对萃取溶剂、衍生化反应温度和时间、衍生试剂(次氯酸钠)的加入量、色谱柱的选择以及色谱分析条件进行了优化,采取正己烷作为萃取试剂,加入次氯酸钠溶液2.0 mL,选择衍生化反应温度为35℃,反应时间为50 min,DB-5细管柱(30 m×0.32 mm,0.25μm)作为分离柱,当取样体积为10 mL时,方法检出限为0.2μg/L。用该方法对实验用水做了高、中、低质量浓度水平的加标回收试验,回收率为85.5%~105.6%,相对标准偏差为2.93%~4.49%(n=6)。A derivatization liquid-liquid extraction gas chromatography method was established for the determination of picric acid in environmental water.The extraction solvent,derivatization reaction temperature and time,addition amount of derivatization reagent(sodium hypochlorite),selection of chromatographic column,and chromatographic analysis conditions were optimized.Using n-hexane as an extraction reagent,add 2.0 mL of sodium hypochlorite solution,select a derivatization reaction temperature of 35℃,a reaction time of 50 min,and DB-5 thin tube column(30 m×0.32 mm,0.25μm)was used as gas chromatography column for analysis.When the sampling volume was 10 mL,the detection limit of the method was 0.2μg/L.The method was used to do the standard addition recovery test of high,medium and low mass concentration levels for the experimental water.The recoveries were 85.5%-105.6%,and the relative standard deviations were 2.93%-4.49%(n=6).

关 键 词：衍生化-液液微萃取 气相色谱法 环境水体 苦味酸 

分 类 号：O657.7[理学—分析化学]