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用于估算氯吡脲残留量的简单高效分析方法的验证。

Validation of simple and efficient analytical methodology for estimation of forchlorfenuron residues.

作者信息

Sharma Neeraj, Sharma Smriti, Mandal Kousik

机构信息

Pesticide Residue Analysis Laboratory, Department of Entomology, Punjab Agricultural University, Ludhiana, 141004, Punjab, India.

出版信息

Environ Monit Assess. 2022 Nov 4;195(1):68. doi: 10.1007/s10661-022-10647-y.

Abstract

A simple and efficient analytical methodology was standardised for the estimation of forchlorfenuron residues in rice leaves, grains, husk, straw and soil using LC-MS/MS. The methodology was validated in terms selectivity, sensitivity, linearity, limit of detection, limit of quantification, matrix effect, repeatability and reproducibility. The limit of detection and limit of quantification of forchlorfenuron in rice leaves, grains, straw, husk and soil were worked out to be 0.003 and 0.01 mg kg, respectively. Recoveries ranged between 81.54 and 99.05% with RSD below 4.57 and RSD below 4.19%. This validated method was applied for the determination of forchlorfenuron residues in paddy leaves after foliar application. The residues persisted for 0, 3 and 7 days after application of forchlorfenuron 0.12% EC @ 1.25, 2.50 and 5.00 ppm a.i. The half-life values were estimated to be 1.91 and 2.11 days for 2.50 and 5.00 ppm a.i. concentration. The residues were found to be below the limit of quantification of 0.01 mg kg in straw, grain, husk and soil samples collected at harvest time.

摘要

建立了一种简单高效的分析方法,用于使用液相色谱 - 串联质谱法(LC-MS/MS)测定水稻叶片、谷粒、稻壳、稻草和土壤中的氯吡脲残留量。该方法在选择性、灵敏度、线性、检测限、定量限、基质效应、重复性和再现性方面进行了验证。水稻叶片、谷粒、稻草、稻壳和土壤中氯吡脲的检测限和定量限分别为0.003和0.01 mg/kg。回收率在81.54%至99.05%之间,相对标准偏差(RSD)低于4.57%,且在不同基质中RSD低于4.19%。该验证方法用于叶面喷施后水稻叶片中氯吡脲残留量的测定。在喷施0.12%乳油,有效成分浓度为1.25、2.50和5.00 ppm的氯吡脲后,残留量分别在0、3和7天进行检测。对于2.50和5.00 ppm有效成分浓度,半衰期值估计分别为1.91和2.11天。在收获时采集的稻草、谷粒、稻壳和土壤样品中,残留量低于0.01 mg/kg的定量限。

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