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农药制剂中甲胺磷、涕灭威和甲维盐的测定:单实验室验证。

Determination of Acephate, Dinotefuran, and Emamectin Benzoate in a Pesticide Formulation: A Single-Laboratory Validation.

机构信息

D. D. N. Bhole College, Bhusawal, Jalgaon, Maharashtra 425 201, India.

Indofil Industries Limited, Thane, Maharashtra 400 607, India.

出版信息

J AOAC Int. 2023 May 3;106(3):523-533. doi: 10.1093/jaoacint/qsad007.

DOI:10.1093/jaoacint/qsad007
PMID:36645232
Abstract

BACKGROUND

The advantage of simultaneous separation and quantification is the reduction of analysis time and consumption of solvents and reagents.

OBJECTIVE

The objective of the present investigation was to optimize and validate a novel, rapid, and simple reverse-phase high-performance liquid chromatographic method for the simultaneous determination of acephate, dinotefuran, and emamectin benzoate in a pesticide formulation.

METHOD

The chromatographic separation and quantification were accomplished by using Kromasil CN column (250 mm × 4.6 mm; 5 μm) with a mobile phase consisting of acetonitrile and water [0.1% (v/v) triethylamine, pH 2.7 with 10% (v/v) orthophosphoric acid] in the ratio of 50:50 (v/v) with a flow rate of 1.0 mL/min and diode array detection at the wavelength of (215 nm and 245 nm).

RESULTS

The HPLC method was able to separate and quantify all the actives in the formulation by isocratic elution within 10 min. The method was fully validated in accordance with the SANCO and Collaborative International Pesticide Analytical Council guidelines concerning system suitability, specificity, linearity, precision, accuracy, and robustness. All the analytical parameters are within the range of acceptable limits in the guidelines.

CONCLUSIONS

The validated method was successfully applied to a pesticide formulation.

HIGHLIGHTS

The novelty of the current research work lies in the development of the simple and rapid HPLC method for simultaneous determination of acephate, dinotefuran, and emamectin benzoate in wettable granular formulation.

摘要

背景

同时分离和定量的优势在于减少了分析时间以及溶剂和试剂的消耗。

目的

本研究的目的是优化和验证一种新的、快速且简单的反相高效液相色谱法,用于同时测定一种农药制剂中的乙酰甲胺磷、噻虫嗪和甲氨基阿维菌素苯甲酸盐。

方法

采用 Kromasil CN 柱(250mm×4.6mm,5μm),以乙腈和水[0.1%(v/v)三乙胺,pH2.7 用 10%(v/v)磷酸调至]为流动相,比例为 50:50(v/v),流速为 1.0mL/min,二极管阵列检测波长为(215nm 和 245nm),完成色谱分离和定量。

结果

该 HPLC 方法能够通过等度洗脱在 10min 内分离和定量配方中的所有活性成分。该方法按照 SANCO 和协作国际农药分析理事会的指南进行了全面验证,涉及系统适用性、专属性、线性、精密度、准确度和稳健性。所有分析参数均在指南规定的可接受范围内。

结论

该验证方法成功应用于农药制剂。

重点

本研究工作的新颖之处在于开发了一种简单快速的 HPLC 方法,用于同时测定可湿性粒剂中乙酰甲胺磷、噻虫嗪和甲氨基阿维菌素苯甲酸盐的含量。

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