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甘蔗和土壤中敌草隆的联合测定方法:超声辅助萃取、碳纳米管介导的净化及气相色谱 - 电子捕获检测

Combined Approach for Determining Diuron in Sugarcane and Soil: Ultrasound-Assisted Extraction, Carbon Nanotube-Mediated Purification, and Gas Chromatography-Electron Capture Detection.

机构信息

College of Food and Biochemical Engineering, Guangxi Science and Technology Normal Univ., Laibin, Guangxi, 546199, China.

出版信息

J Food Sci. 2019 Sep;84(9):2402-2411. doi: 10.1111/1750-3841.14752. Epub 2019 Aug 20.

Abstract

Diuron is a urea herbicide that is frequently detected in surface water, groundwater, and marine waters. However, there are few methods or guidelines reported on ensuring the quality of sugarcane and soil. In this study, a method was developed for detecting diuron to ensure the quality and safety of food and sugar. Mass spectrometry was used to identify 3,4-dichloroaniline as a marker for the thermal decomposition of diuron, and thus, as a representative component for quantitative diuron analysis. This approach can be used to rapidly detect trace amounts of diuron. In addition, ultrasound-assisted extraction (UAE) and carbon nanotube column purification were used in conjunction with gas chromatography-electron capture detection to detect diuron. The method was then evaluated for its accuracy, detection limit, and viability. The effects of extraction solvent, ultrasound time, and ultrasound power on the extraction efficiency of the analyte from sugarcane and soil were also investigated. The efficiency and optimum conditions of UAE were examined through single-factor experiments and Box-Behnken design (BBD). The optimal extraction conditions were identified as follows: acetonitrile as the extraction solvent, extraction temperature of 27 °C, extraction time of 3.4 min, and ultrasound power of 70 W. Under these conditions, high linearity was achieved for diuron concentrations of 0.01 to 5.0 mg/L, and the purification correlation coefficient was consistently greater than 0.998. Hence, gas chromatography, combined with UAE and BBD, offers superior efficiency extraction, which is sufficiently accurate and precise for pesticide residue analysis. PRACTICAL APPLICATION: We developed an accurate and cost-effective method for detecting diuron (a commonly used herbicide) in soil and sugar samples. We performed experiments to determine the optimum detection conditions for our method. This method can be used for online monitoring of sugar manufacturing processes to ensure food safety and quality.

摘要

敌草隆是一种尿素类除草剂,经常在地表水、地下水和海水中被检测到。然而,关于确保甘蔗和土壤质量的方法或指南报道较少。在本研究中,开发了一种检测敌草隆的方法,以确保食品和糖的质量与安全。采用质谱法鉴定3,4-二氯苯胺作为敌草隆热分解的标志物,因此作为定量分析敌草隆的代表性成分。该方法可用于快速检测痕量敌草隆。此外,将超声辅助萃取(UAE)和碳纳米管柱净化与气相色谱 - 电子捕获检测相结合来检测敌草隆。然后对该方法的准确性、检测限和可行性进行评估。还研究了萃取溶剂、超声时间和超声功率对从甘蔗和土壤中萃取分析物效率的影响。通过单因素实验和Box-Behnken设计(BBD)研究了UAE的效率和最佳条件。确定的最佳萃取条件如下:乙腈作为萃取溶剂,萃取温度为27℃,萃取时间为3.4分钟,超声功率为70W。在这些条件下,敌草隆浓度在0.01至5.0mg/L范围内具有高线性,净化相关系数始终大于0.998。因此,气相色谱结合UAE和BBD提供了高效萃取,对农药残留分析具有足够的准确性和精密度。实际应用:我们开发了一种准确且经济高效的方法来检测土壤和糖样品中的敌草隆(一种常用除草剂)。我们进行了实验以确定该方法的最佳检测条件。该方法可用于制糖过程的在线监测,以确保食品安全和质量。

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