Malhat Farag, Abdallah Osama I, Saber El-Sayed, Ahmed Nevein S, Salam Shokr Shokr Abdel
Pesticide Residues and Environmental Pollution Department, Central Agricultural Pesticide Laboratory, Agricultural Research Center Dokki Giza 12618 Egypt
RSC Adv. 2025 Mar 3;15(9):6688-6699. doi: 10.1039/d5ra00176e. eCollection 2025 Feb 26.
This study developed and validated an LC-MS/MS analytical method for determining abamectin and fenpyroximate residues in okra fruits. The method optimization focused on chromatographic separation and ionization conditions, adding formic acid and ammonium formate to enhance ionization efficiency and signal sensitivity. Validation was performed according to SANTE guidelines, demonstrating good selectivity, linearity ( > 0.998), precision, recovery, and minimal matrix effects (14.6% for abamectin and 5.2% for fenpyroximate). The limit of detection (LOD) was set at 0.0006 mg kg for abamectin and 0.0002 mg kg for fenpyroximate, while the limit of quantification (LOQ) was 0.002 mg kg and 0.001 mg kg, respectively. Precision was within acceptable limits, with intra-day RSD of 11.4% for abamectin and 7.6% for fenpyroximate. Recovery ranged from 84.2% to 98.6%, meeting the acceptable 70-120% range. Persistence studies indicated that abamectin and fenpyroximate residues dissipated over time, with half-lives of 2.3 and 2.45 days, respectively. The pre-harvest interval (PHI) required for residues to fall below the maximum residue limit (MRL) was estimated to be 2.6 days for abamectin and 6.9 days for fenpyroximate. The risk quotient was assessed based on the Egyptian adult consumers' consumption of okra, ensuring a negligible risk.
本研究建立并验证了一种用于测定秋葵果实中阿维菌素和唑螨酯残留量的液相色谱-串联质谱(LC-MS/MS)分析方法。该方法优化主要集中在色谱分离和电离条件上,通过添加甲酸和甲酸铵来提高电离效率和信号灵敏度。根据SANTE指南进行了验证,结果表明该方法具有良好的选择性、线性(>0.998)、精密度、回收率,且基质效应极小(阿维菌素为14.6%,唑螨酯为5.2%)。阿维菌素的检测限(LOD)设定为0.0006 mg/kg,唑螨酯的检测限为0.0002 mg/kg,而定量限(LOQ)分别为0.002 mg/kg和0.001 mg/kg。精密度在可接受范围内,阿维菌素的日内相对标准偏差(RSD)为11.4%,唑螨酯为7.6%。回收率在84.2%至98.6%之间,符合70%-120%的可接受范围。残留研究表明,阿维菌素和唑螨酯残留量随时间消散,半衰期分别为2.3天和2.45天。估计阿维菌素残留量降至最大残留限量(MRL)以下所需的收获前间隔(PHI)为2.6天,唑螨酯为6.9天。基于埃及成年消费者对秋葵的消费量评估了风险商数,确保风险可忽略不计。