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采用 SiO2 微球柱固相萃取对环境水样中的拟除虫菊酯类杀虫剂进行预浓缩敏感测定,然后进行高效液相色谱分析。

Preconcentration sensitive determination of pyrethroid insecticides in environmental water samples with solid phase extraction with SiO2 microspheres cartridge prior to high performance liquid chromatography.

机构信息

School of Chemistry and Environmental Sciences, Henan Normal University, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huaihe River Water Environment and Pollution Control, Ministry of Education, Xinxiang 453007, China.

出版信息

J Chromatogr A. 2010 Jul 30;1217(31):5021-5. doi: 10.1016/j.chroma.2010.05.060. Epub 2010 Jun 4.

Abstract

Present study developed a new method for the sensitive determination of pyrethroid insecticides with solid phase extraction in combination with high performance liquid chromatography and UV detector. SiO(2) microspheres, a new SiO(2) based material, was investigated for the enrichment ability and applicability as the solid phase extraction sorbent. Four pyrethroid pesticides such as fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were used as the target analytes. Parameters that maybe influence the extraction efficiency such as the eluent type and its volume, sample flow rate, sample pH, and the sample volume were optimized in detail, and the optimal conditions were as followed: sample volume, 100mL; concentration of methanol, 30%; acetone volume, 5mL; sample flow rate, 4.2mLmin(-1); sample pH, 7. The experimental results indicated that there was good linearity in the concentration range of 0.1-50microgL(-1) except biphenthrin in the range of 0.05-25microgL(-1). The detection limits for fenpropathrin, cyhalothrin, fenvalevate and biphenthrin were in the range of 0.02-0.08microgL(-1). The intra-day and day to day precisions (RSDs, n=6) were in the ranges of 2.6-4.4% and 5.3-7.2%, respectively. The method was validated with five real environmental water samples, and all these results proved that proposed method could be used as a good alternative for the routine analysis for such pollutants in environmental samples.

摘要

本研究开发了一种新的方法,用于结合高效液相色谱和紫外检测器,通过固相萃取来灵敏地测定拟除虫菊酯类杀虫剂。SiO2 微球,一种新型的 SiO2 基材料,被研究作为固相萃取吸附剂的富集能力和适用性。四种拟除虫菊酯类农药,如氯菊酯、氯氰菊酯、氰戊菊酯和联苯菊酯,被用作目标分析物。详细优化了可能影响萃取效率的参数,如洗脱剂类型和体积、样品流速、样品 pH 值和样品体积,并优化了最佳条件:样品体积为 100mL;甲醇浓度为 30%;丙酮体积为 5mL;样品流速为 4.2mLmin(-1);样品 pH 值为 7。实验结果表明,除联苯菊酯在 0.05-25μg/L 范围内外,在 0.1-50μg/L 的浓度范围内均有良好的线性关系。氯菊酯、氯氰菊酯、氰戊菊酯和联苯菊酯的检测限在 0.02-0.08μg/L 范围内。日内和日间精密度(n=6)分别在 2.6-4.4%和 5.3-7.2%范围内。该方法用 5 个实际环境水样进行了验证,所有这些结果都证明,该方法可作为环境样品中此类污染物常规分析的一种良好替代方法。

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