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<p>In the manufacturing process of pesticide formulations, quality control plays a crucial part in ensuring its effectiveness and meeting requirements of regulatory for safe use. In this paper, a simplified HPLC-based method has been developed for simultaneous quantitative determination of Pyriproxyfen and Bifenthrin in 10% EC formulation using a C-18 analytical column (150&#xa0;mmX4.6&#xa0;mmX5&#xa0;µm). Based on chromatographic separation with good resolution, acetonitrile: water (80:20, v/v) was selected as mobile phase in isocratic mode with a flow rate of 1.2&#xa0;mL/min at a constant column temperature of 30&#xa0;°C and UV detection at 220&#xa0;nm. The method was validated in line with SANCO/3030/99 rev. 5 guidelines encompassing the key parameters system suitability, linearity, precision, recovery, LOD &amp; LOQ. The validation parameters were found within acceptance criteria. The LOD and LOQ for Pyriproxyfen was 8.6&#xa0;mg/L and 26.0&#xa0;mg/L while that of Bifenthrin was 10.0&#xa0;mg/L and 30.0&#xa0;mg/L, respectively. Precision with acceptable %RSD of &lt; 2% and recoveries ranging from 80 to 120% were obtained. Further escorting the decision making and confidence in the reliability of the produced data, measurement uncertainty using Eurachem/ CITAC procedure were obtained. The contributions to the uncertainty of measurement were from sample preparation, calibration standards preparation, calibration curve, and purity data. The contribution to the uncertainty of measurement from the analysis by HPLC were repeatability and intra-lab reproducibility. The combined expanded uncertainty of measurement was between 0.15% and 0.19%. The proposed analytical method is suitable for simultaneous quantitative determination of pyriproxyfen and bifenthrin in respective formulations.</p>

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Method validation of pyriproxyfen and bifenthrin for simultaneous determination in pesticide formulation using simplified reverse phase high-performance liquid chromatography (RP-HPLC) method and estimation of measurement uncertainty

  • 期刊论文

  • 发表日期：

    2025年9月19日

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  • Reema Chaudhary,
  • Rakhi Singh,
  • Prabal Pratap Singh,
  • Mukul Das

摘要

In the manufacturing process of pesticide formulations, quality control plays a crucial part in ensuring its effectiveness and meeting requirements of regulatory for safe use. In this paper, a simplified HPLC-based method has been developed for simultaneous quantitative determination of Pyriproxyfen and Bifenthrin in 10% EC formulation using a C-18 analytical column (150 mmX4.6 mmX5 µm). Based on chromatographic separation with good resolution, acetonitrile: water (80:20, v/v) was selected as mobile phase in isocratic mode with a flow rate of 1.2 mL/min at a constant column temperature of 30 °C and UV detection at 220 nm. The method was validated in line with SANCO/3030/99 rev. 5 guidelines encompassing the key parameters system suitability, linearity, precision, recovery, LOD & LOQ. The validation parameters were found within acceptance criteria. The LOD and LOQ for Pyriproxyfen was 8.6 mg/L and 26.0 mg/L while that of Bifenthrin was 10.0 mg/L and 30.0 mg/L, respectively. Precision with acceptable %RSD of < 2% and recoveries ranging from 80 to 120% were obtained. Further escorting the decision making and confidence in the reliability of the produced data, measurement uncertainty using Eurachem/ CITAC procedure were obtained. The contributions to the uncertainty of measurement were from sample preparation, calibration standards preparation, calibration curve, and purity data. The contribution to the uncertainty of measurement from the analysis by HPLC were repeatability and intra-lab reproducibility. The combined expanded uncertainty of measurement was between 0.15% and 0.19%. The proposed analytical method is suitable for simultaneous quantitative determination of pyriproxyfen and bifenthrin in respective formulations.