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响应面法在利用介孔碳CMK-3优化天然水和生物样品中痕量二嗪农预富集的应用

Application of response surface methodology for optimization of trace amount of diazinon preconcentration in natural waters and biological samples by carbon mesoporous CMK-3.

作者信息

Beirami Somayeh, Barzoki Hadi Rahimzadeh, Bahramifar Nader

机构信息

Environmental Health Research Center, Golestan University of Medical Sciences, Gorgan, Iran.

Environmental Health Research Center, Golestan University of Medical Sciences, Gorgan, Iran and Environmental Health Engineering Department, Hamedan University of Medical Science, Hamedan, Iran.

出版信息

Biomed Chromatogr. 2017 May;31(5). doi: 10.1002/bmc.3874. Epub 2017 Jan 19.

Abstract

Preconcentration of trace amounts of diazinon by carbon mesoporous CMK-3 in water and biological samples and measurement by high-performance liquid chromatography were investigated. CMK-3 was prepared using hexagonal SBA-15 as the template. The synthesized materials were characterized by X-Ray diffraction (XRD), Fourier transform infrared spectroscopy, Brunaur-Emmet-Teller, transmission electron microscopy and Boehm titration method. The preconcentration procedure was optimized using a multivariate optimization approach following a two-stage process. The effect of analytical parameters including the amount of the CMK-3 as an adsorbent, pH, type and volume of eluent and flow rate of eluent and sample were studied by a screening project, then the effective parameters were optimized by response surface methodology based on central composite design. The average extraction efficiency of diazinon under optimal conditions (CMK-3 dosage = 25 mg, sample flow rate = 2.5 mL min , eluent flow rate = 1.25 mL min , volume of methanol as an eluent =3.5 mL and initial pH = 6) was 97.11%, which agrees well with the predicted response value (97.93%). The linearity of the method was in the range of 0.5-100 μg L with a correlation coefficient of 0.997. Enrichment factor, limit of detection and limit of quantification were 285.7, 0.09 and 0.23 μg L , respectively. The relative standard deviation (RSD) under optimum conditions was 2.21% (n = 5). The proposed method was applied to determine diazinon in real water and biological samples. Recovery of diazinon from real samples was between 95.80 and 104.94% with an RSD of 0.19-4.65%. Thus, this method is suitable for the preconcentration and determination of diazinon in real water and biological samples.

摘要

研究了采用介孔碳CMK-3对水和生物样品中的痕量二嗪农进行预富集,并通过高效液相色谱法进行测定。以六方SBA-15为模板制备CMK-3。采用X射线衍射(XRD)、傅里叶变换红外光谱、布鲁诺尔-埃米特-泰勒法、透射电子显微镜和 Boehm滴定法对合成材料进行了表征。采用多变量优化方法分两阶段对预富集过程进行了优化。通过筛选实验研究了分析参数的影响,包括作为吸附剂的CMK-3用量、pH值、洗脱剂的类型和体积、洗脱剂和样品的流速,然后基于中心复合设计采用响应面法对有效参数进行了优化。在最佳条件下(CMK-3用量 = 25 mg,样品流速 = 2.5 mL min,洗脱剂流速 = 1.25 mL min,甲醇洗脱剂体积 = 3.5 mL,初始pH = 6)二嗪农的平均萃取效率为97.11%,与预测响应值(97.93%)吻合良好。该方法的线性范围为0.5 - 100 μg L,相关系数为0.997。富集因子、检测限和定量限分别为285.7、0.09和0.23 μg L。最佳条件下的相对标准偏差(RSD)为2.21%(n = 5)。该方法用于实际水和生物样品中二嗪农的测定。实际样品中二嗪农的回收率在95.80%至104.94%之间,RSD为0.19% - 4.65%。因此,该方法适用于实际水和生物样品中二嗪农的预富集和测定。

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