Ding W H, Lo J H, Tzing S H
Department of Chemistry, National Central University, Chung-Li, Taiwan.
J Chromatogr A. 1998 Sep 4;818(2):270-9. doi: 10.1016/s0021-9673(98)00550-0.
A method was developed for the analysis of linear alkylbenzenesulfonates (LAS) and their degradation products, sulfophenylcarboxylic acids (SPC), in samples of sewage effluent and river water. This method involved extraction of the samples by graphitized carbon black cartridge, esterification by a two-step thionyl chloride-trifluoroethanol derivatization procedure, and separation, identification and quantitation by ion-trap GC-MS with EI and low pressure CI modes. High selectivity with few signals was observed in the low pressure CI mass spectra of LAS and SPC. Enhanced sensitivity with protonated molecular ion chromatograms of homologous C10-C13 LAS by CI-MS permit the determination of LAS and SPC at trace concentrations in environmental samples. Recovery rates of LAS and SPC in spiked water samples ranged from 75 to 112% with R.S.D. values from 3 to 26%. The limit of quantitation for both LAS and SPC was estimated to be 0.01 microgram/l in 100 ml of water sample.
开发了一种分析污水和河水样品中直链烷基苯磺酸盐（LAS）及其降解产物磺基苯基羧酸（SPC）的方法。该方法包括用石墨化炭黑柱提取样品，通过两步亚硫酰氯 - 三氟乙醇衍生化程序进行酯化，以及采用电子轰击电离（EI）和低压化学电离（CI）模式的离子阱气相色谱 - 质谱联用仪进行分离、鉴定和定量。在LAS和SPC的低压CI质谱中观察到信号少的高选择性。通过CI - MS对同源C10 - C13 LAS的质子化分子离子色谱图增强了灵敏度，从而能够测定环境样品中痕量浓度的LAS和SPC。加标水样中LAS和SPC的回收率在75%至112%之间，相对标准偏差（R.S.D.）值在3%至26%之间。估计在100 ml水样中LAS和SPC的定量限均为0.01微克/升。
