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采用 C18毛细管整体柱作为固相微萃取整体柱,构建在线固相微萃取-高效液相色谱联用系统,同步富集检测环境水样中的5种苯氧羧酸类除草剂。详细考察了联用系统运行条件对富集检测的影响。联用系统运行最佳参数为:固相微萃取整体柱长度20 cm,进样流速0.04 mL/min,进样13 min,洗脱流速0.02 mL/min,洗脱5 min。在最佳条件下,5种苯氧羧酸类除草剂的检出限为:9μg/L(苯氧丙酸)、4μg/L(2-(2-氯)-苯氧丙酸)、4μg/L(2-(3-氯)-苯氧丙酸)、5μg/L(2,4-二氯苯氧乙酸)、5μg/L(2-(2,4-二氯苯氧基)丙酸)。与 HPLC 系统直接进样对比,联用系统对5种检测对象表现出优良的富集能力。5种苯氧羧酸类除草剂的回收率在79.0%~98.0%之间( RSD≤3.9%)。该方法成功应用于水样中5种苯氧羧酸类除草剂的检测,结果令人满意。

A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides,including 2,4-dichlorophenoxyacetic acid(2,4-D),2-(2-chloro)-phenoxy propionic acid(2,2-CPPA),2-(3-chloro)-phenoxy propionic acid(2,3-CPPA),phenoxy propionic acid(PPA)and 2-(2,4-dichlorophenoxy)propionic acid(2,4-DP). The operating parameters of the in-tube SPME-HPLC system ,including the length of the mono-lithic column,the sampling flow rate,the sampling time,the elution flow rate and the elution time,had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow:the length of the monolithic column was 20 cm,the sampling flow rate was 0. 04 mL/min, sampling time was 13 min;the elution flow rate was 0. 02 mL/min,elution time was 5 min. Under the optimized conditions,the detection limits of the five phenoxy acid herbicides were as follows:9 μg/L for PPA,4 μg/L for 2,2-CPPA,4 μg/L for 2,3-CPPA,5 μg/L for 2,4-D,5 μg/L for 2,4-DP. Compared with the HPLC method with di-rect injection,the combined system showed a good enrichment factors to the analytes. The re-coveries of the five phenoxy acid herbicides were between 79. 0% and 98. 0%( RSD≤3. 9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.

参考文献

[1] Wang,J.;Jia,W.;Lin,X.;Wu,X.;Xie,Z..Phenylalanine functionalized zwitterionic monolith for hydrophobic interaction electrochromatography[J].Electrophoresis: The Official Journal of the International Electrophoresis Society,201324(24):3293-3299.
[2] Lin J;Wu XP;Lin XC;Xie ZH.Preparation of polymethacrylate monolithic stationary phases having bonded octadecyl ligands and sulfonate groups: Electrochromatographic characterization and application to the separation of polar solutes for pressurized capillary electrochromatogra[J].Journal of chromatography, A: Including electrophoresis and other separation methods,20071/2(1/2):220-227.
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