固相膜萃取-超声洗脱衍生法分析水中酚类化合物

建立了水中酚类化合物的新型预处理技术。在水样pH 3~4时，采用SDB-XC固相萃取膜，5 min可完成500 mL水样中酚类化合物的萃取；将膜片折叠置于反应瓶中，以五氟苄基溴溶液为衍生试剂，20 min可完成膜片上酚类化合物的超声洗脱和衍生；以HP-5MS色谱柱（30 m×0.25 mm×0.25 μm）为分析柱，用负化学电离源在10 min内完成检测。对膜片的选择、酸度的控制、衍生条件、超声条件及干扰情况进行逐一分析并优化，结果表明，在10~200 μg/L线性范围内，各组分的相关系数r²>0.997，加标回收率在70%~107%之间，相对标准偏差为3.8%~10.4%。应用该方法检测实际样品，部分样品有检出。该方法可实现样品的快速萃取、洗脱衍生一体化、低污染和高灵敏检测。

Determination of Phenolic Compounds in Water by Solid Phase Membrane Extraction Coupled with Ultrasonic Assisted Desorption and Derivation

A new pretreatment technology of phenolic compounds analysis in water was established. When the pH value of the water sample was 3-4, the extraction of phenolic compounds in 500 mL water sample could be completed in 5 min by using SDB-XC solid phase extraction membrane. Then the folded membrane was put into a reaction bottle, in which five fluorinated benzyl bromide solution was used as the derivatization reagent to complete the elution and derivatization of phenolic compounds on the membrane by 20 min ultrasound. HP-5MS column （30 m×0.25 mm×0.25 μm） was selected as analytical column, the detection could be completed within 10 min by using negative chemical ionization source. In this method, the selection of membrane, the control of acidity, derivation condition, ultrasonic condition and interference situation were analyzed and optimized. The results showed that the correlation coefficient of each component was greater than 0.997 in the linear range of 10-200 μg/L. The recoveries of different concentrations were 70%-107%, and the relative standard deviations were 3.8%-10.4%. Some phenolic compounds were detected in actual samples by this method. The method can achieve the rapid extraction, synchronous elution, low pollution and high sensitivity detection of samples.