Application of SiO2 hollow fibers for sorptive microextraction and gas chromatography–mass spectrometry determination of organochlorine pesticides in herbal matrices
Application of SiO2 hollow fibers for sorptive microextraction and gas chromatography–mass spectrometry determination of organochlorine pesticides in herbal matrices
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DOI：
10.1007/s00216-010-4025-9
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发表时间：
2010-07
影响因子：
4.3
通讯作者：
Jia Li;Hong-fei Zhang;Yan-ping Shi
中科院分区：
文献类型：
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作者：
Jia Li;Hong-fei Zhang;Yan-ping Shi
描述了一种涉及同时提取和样品净化程序的方法：中空纤维吸附微萃取，结合气相色谱-质谱检测，对大黄中的七种有机氯农药进行定量。首次合成了具有多孔结构的SiO2中空纤维。 SiO2中空纤维的内径为380μm，平均壁厚为100μm。聚集的SiO2颗粒以规则排列沉积在中空纤维表面，形成多孔结构。将SiO2中空纤维应用于大黄中有机氯农药的测定，可避免样品净化并最大限度地减少基质效应。对萃取溶剂、萃取温度和平衡时间进行了优化。浓度范围内纤维间的重复性小于 10%。大多数有机氯农药在加标水平下的回收率令人满意（63% 至 115%）。此外，该方法还用于测定43个市售大黄样品中的7种有机氯农药，其中8个样品中发现了所选农药。采用中国药典（2005年版）溶剂萃取法进一步证实了该结果。图SiO2中空纤维提取大黄中有机氯农药的GC-MS-SIM色谱图（插图为SiO2中空纤维SEM）。
A method involving simultaneous extraction and sample clean-up procedure: hollow fiber sorptive microextraction, coupled with gas chromatography–mass spectrometric detection for quantification of seven organochlorine pesticides in Radix et Rhizoma Rhei is described. SiO2hollow fiber with porous structure was synthesized for the first time. The internal diameter of SiO2hollow fiber is 380 μm and average wall thickness is 100 μm. Aggregated SiO2particles deposited on the surface of the hollow fiber in a regular array lead to porous structure. SiO2hollow fiber was applied to the determination of organochlorine pesticides in Radix et Rhizoma Rhei to avoid sample clean-up and minimize the matrix effects. Extraction solvent, extraction temperature and equilibration time were optimized. Fiber to fiber repeatability over the concentration ranges were less than 10%. Recoveries were satisfactory (between 63% and 115%) for most of organochlorine pesticides at spiking levels. Furthermore, the proposed method was also applied to determine seven organochlorine pesticides in 43 commercial Radix et Rhizoma Rhei samples, in which the selected pesticides were found in eight samples. The results have been further confirmed by solvent extraction methods according to China Pharmacopoeia (2005).FigureGC-MS-SIM chromatograms of organochlorine pesticides in Radix et Rhizoma Rhei extracted with SiO2hollow fibers (insetSEM of SiO2hollow fiber).