新型溶胶-凝胶杂化甲基三甲氧基硅烷-四乙氧基硅烷作为固相萃取吸附剂用于有机磷农药。
Novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides.
机构信息
Separation Science and Technology Group, Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia.
出版信息
J Chromatogr A. 2012 Mar 16;1229:55-62. doi: 10.1016/j.chroma.2012.01.022. Epub 2012 Jan 18.
A novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was produced and applied as sorbent for solid phase extraction (SPE). Five selected organophosphorus pesticides (OPPs) were employed as model compounds to evaluate the extraction performance of the synthesized sol-gel organic-inorganic hybrid MTMOS-TEOS. Analysis was performed using gas chromatography-mass spectrometry. Several important SPE parameters were optimized. Under the optimum extraction conditions, the method using the sol-gel organic-inorganic hybrid MTMOS-TEOS as SPE sorbent showed good linearity in the range of 0.001-1 μg L(-1), good repeatability (RSD 2.1-3.1%, n=5), low limits of detection at S/N=3 (0.5-0.9 pg mL(-1)) and limit of quantification (1-3 pg mL(-1), S/N=10). The performance of the MTMOS-TEOS SPE was compared to commercial C18 Supelclean SPE since C18 SPE is widely used for OPPs. The MTMOS-TEOS SPE method LOD was 500-600 × lower than the LOD of commercial C18 SPE. The LOD achieved with the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent allowed the detection of these OPPs in drinking water well below the level set by European Union (EU) at 0.1 μg L(-1) of each pesticides. The developed MTMOS-TEOS SPE method was successfully applied to real sample analysis of the selected OPPs from several water samples and its application extended to the analysis of several fruits samples. Excellent recoveries and RSDs of the OPPs were obtained from the various water samples (recoveries: 97-111%, RSDs 0.4-2.8%, n=3) and fruit samples (recoveries: 96-111%), RSDs 1-4%, n=5) using the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent. Recoveries and RSDs of OPPs from river water samples and fruit samples using C18 Supelclean SPE sorbent were 91-97%, RSD 0.9-2.6, n=3 and 86-96%, RSD 3-8%, n=5, respectively). The novel sol-gel hybrid MTMOS-TEOS SPE sorbent demonstrate the potential as an alternative inexpensive extraction sorbent for OPPs with higher sensitivity for the OPPs.
一种新型溶胶-凝胶杂化甲基三甲氧基硅烷-四乙氧基硅烷（MTMOS-TEOS）被制备并用作固相萃取（SPE）的吸附剂。选择五种有机磷农药（OPPs）作为模型化合物来评估合成的溶胶-凝胶有机-无机杂化 MTMOS-TEOS 的萃取性能。使用气相色谱-质谱法进行分析。优化了几个重要的 SPE 参数。在最佳萃取条件下，使用溶胶-凝胶有机-无机杂化 MTMOS-TEOS 作为 SPE 吸附剂的方法在 0.001-1μg L(-1) 范围内具有良好的线性关系，具有良好的重现性（RSD 2.1-3.1%，n=5），检测限低至 S/N=3（0.5-0.9 pg mL(-1)) 和定量限（1-3 pg mL(-1), S/N=10)。MTMOS-TEOS SPE 的性能与商业 C18 Supelclean SPE 进行了比较，因为 C18 SPE 广泛用于 OPPs。MTMOS-TEOS SPE 方法的 LOD 比商业 C18 SPE 的 LOD 低 500-600 倍。使用溶胶-凝胶有机-无机杂化 MTMOS-TEOS SPE 吸附剂实现的 LOD 允许在饮用水中检测到这些 OPPs，其浓度远低于欧盟（EU）设定的 0.1μg L(-1) 每种农药的水平。开发的 MTMOS-TEOS SPE 方法成功应用于从几种水样中选择的 OPPs 的实际样品分析，并将其应用扩展到几种水果样品的分析。使用溶胶-凝胶有机-无机杂化 MTMOS-TEOS SPE 吸附剂，从各种水样（回收率：97-111%，RSD 0.4-2.8%，n=3）和水果样品（回收率：96-111%）中获得了 OPPs 的良好回收率和 RSDs%，RSD 1-4%，n=5）。使用 C18 Supelclean SPE 吸附剂从河水样和水果样中回收 OPPs 的回收率和 RSD 分别为 91-97%，RSD 0.9-2.6，n=3 和 86-96%，RSD 3-8%，n=5）。新型溶胶-凝胶杂化 MTMOS-TEOS SPE 吸附剂具有作为 OPPs 更高灵敏度的替代廉价萃取吸附剂的潜力。
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