Tripathy Vandana, Saha Ajoy, Patel Dilipkumar J, Basak B B, Shah Paresh G, Kumar Jitendra
a ICAR-Directorate of Medicinal and Aromatic Plants Research , Anand , Gujarat , India.
b Pesticide Residue Laboratory, Anand Agricultural University , Anand , Gujarat , India.
J Environ Sci Health B. 2016 Aug 2;51(8):508-18. doi: 10.1080/03601234.2016.1170544. Epub 2016 May 6.
A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.
建立了一种基于改良QuEChERS（快速、简便、廉价、高效、耐用和安全）方法的简单多残留方法，用于测定印度一种具有重要经济价值的药用植物番泻叶（决明子）中的17种有机氯（OC）、15种有机磷（OP）和7种拟除虫菊酯（SP）类农药，采用气相色谱联用电子捕获和火焰热离子检测器（GC/ECD/FTD），并通过气相色谱-质谱联用仪（GC-MS）对残留进行确证。通过测试以下参数对所建立的方法进行验证：线性、检测限（LOD）、定量限（LOQ）、基质效应、准确度-精密度和测量不确定度；验证研究清楚地证明了该方法适用于其预期应用。所有农药在0.01-1.0 μg mL⁻¹范围内对OCs和OPs以及在0.05-2.5 μg mL⁻¹范围内对SPs均表现出良好的线性，相关系数高于0.98。该方法对大多数农药的回收率良好（70-120%），在大多数情况下日内和日间精密度<20%。检测限在0.003至0.03 mg kg⁻¹之间，定量限确定为0.01-0.049 mg kg⁻¹。扩展不确定度<30%，明显低于±50%的最大默认值。所提出的方法成功应用于测定从印度不同地点获得的12个商业市场样品中的农药残留。
