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采用响应面法优化分子印迹聚合物移液器吸头微固相萃取后测定海水和食品样品中的丙溴磷。

Determination of profenofos in seawater and foodstuff samples after its molecularly imprinted polymer pipette-tip micro solid phase extraction optimized by response surface methodology.

作者信息

Tamandani Mahsa, Hashemi Sayyed Hossein, Kaykhaii Massoud, Jamali Keikha Ahmad, Nasiriyan Ali

机构信息

Department of Marine Chemistry, Faculty of Marine Science, Chabahar Maritime University, Chabahar, Iran.

Department of Process Engineering and Chemical Technology, Faculty of Chemistry, Gdansk University of Technology, G. Narutowicza St. 11/12, 80-233, Gdansk, Poland.

出版信息

BMC Chem. 2022 Mar 15;16(1):12. doi: 10.1186/s13065-022-00807-z.

Abstract

BACKGROUND

In this research, a molecularly imprinted polymer (MIP) was synthesized and employed as a sorbent for pipette-tip micro solid phase extraction of profenofos insecticide in seawater, rice, and fish samples. The instrument employed for quantitation was spectrophotometry.

RESULTS

Various factors affecting the microextraction protocol, including type and volume of the elution solvent, weight of MIP, pH and volume of sample solution, and number of cycles of loading and desorption were considered and optimized using one-factor-at-a-time, central composite design and Box-Behnken design. Factors optimized at: pH 4.0, amount of sorbent 2.5 mg, volume of methanol:acetic (9:1) acid as eluent 250 µL, both the number of extraction and elution cycles 5, and volume of sample 8.0 mL. At optimized conditions, an enrichment factor of 31 was achieved and the linearity range of the method was between 1.0 and 1000.0 µg/L. A good detection limit of 0.33 µg/L with a reproducibility better than 5.6% (as RSD) was observed.

CONCLUSION

The technique showed good analytical features for determination of profenofos in seawater, rice, and fish samples. Simplicity of operation of spectrophotometry and lack of using expensive HPLC grade solvents are other points of strengths of this method. The total analysis time was about 10 min, which is far less than techniques such as HPLC. Comparison between optimization with central composite design and Box-Behnken design showed better performance of the former.

摘要

背景

在本研究中,合成了一种分子印迹聚合物(MIP),并将其用作吸附剂,用于对海水、大米和鱼类样品中的丙溴磷杀虫剂进行移液器吸头微固相萃取。用于定量的仪器是分光光度计。

结果

考虑了影响微萃取方案的各种因素,包括洗脱溶剂的类型和体积、MIP的重量、样品溶液的pH值和体积以及加载和解吸的循环次数,并采用单因素法、中心复合设计和Box-Behnken设计进行了优化。优化后的因素为:pH 4.0,吸附剂用量2.5mg,甲醇:乙酸(9:1)作为洗脱剂的体积250μL,萃取和洗脱循环次数均为5次,样品体积8.0mL。在优化条件下,富集因子为31,该方法的线性范围为1.0至1000.0μg/L。观察到良好的检测限为0.33μg/L,重现性优于5.6%(相对标准偏差)。

结论

该技术在测定海水、大米和鱼类样品中的丙溴磷方面显示出良好的分析特性。分光光度法操作简单且不使用昂贵的HPLC级溶剂是该方法的其他优点。总分析时间约为10分钟,远少于HPLC等技术。中心复合设计和Box-Behnken设计的优化比较表明前者性能更好。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f297/8922791/2dcab2f92cb6/13065_2022_807_Fig1_HTML.jpg

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