GC/EI-MS and UV-Vis analysis of pesticide residues in cultivated Catha edulis Forsk (Khat) from selected farms in Meru County, Kenya

A. M. Oyugi, Jonathan O. Adongo, C. M. Mudalungu, J. Kibet
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Abstract

In this study, an analysis of pesticide residues was performed using a gas chromatography/ electron impact mass spectrometer (GC/EI-MS) to qualitatively assess and characterize pesticide residues in khat leaves sampled from selected agricultural farms in Meru County, Kenya. A solid-phase microextraction (SPME) procedure followed by GC/EI-MS analysis led to the detection and identification of six pesticide compounds from the sample-ion chromatograms. They include cypermethrin, acephate, cyhalothrin, cyfluthrin, chlorpyrifos, and chlorfenvinphos. The prevalence rate of pesticide contamination was determined to be 54.5% of the sample size. Of the identified pesticide residues, 50% were compounds based on pyrethroids and the other 50% were based on organophosphate. Four of the six identified pesticides were chlorinated compounds. A quick, easy, cheap, effective, rugged, and safe UV-vis double beam spectrophotometric technique based on copper (II) chelation reactions leading to colored copper pesticide complexes was developed, validated, and applied to quantify and compare the levels of selected pesticide compounds found in the khat samples. UV-vis wavelength-scan measurements performed on pesticide compounds chelated with copper (II) ions revealed maximum absorption of Cu-cypermethrin and Cu-acephate at 321 and 207 nm, respectively. The standards calibration curves developed from the UV-Vis quantitation technique showed excellent linearity in the concentration range of 0.5-10.0 µg/L (R2 = 0.99) for both cypermethrin and acephate standards. The estimated limits of quantification (LOQ) were 0.25-0.26 µg/L, respectively. The UV-Vis quantitation results from the selected samples (in which residues were confirmed to be present) revealed that acephate (an organophosphate residue) occurred at higher concentration levels (range 2.897-7.978 µg/L) than cypermethrin (2.145 µg/L). For the pesticides quantitatively analysed in the selected samples, the levels were below the maximum residue limit (MRL). The hazard quotients (HQ) were in the range of between 0.247-0.797.
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肯尼亚梅鲁县部分养殖场栽培杜香中农药残留的GC/EI-MS和UV-Vis分析
在这项研究中,使用气相色谱/电子冲击质谱仪(GC/EI-MS)对农药残留进行了分析,以定性评估和表征从肯尼亚梅鲁县选定的农业农场取样的卡塔叶中的农药残留。固相微萃取(SPME)程序,然后进行GC/EI-MS分析,从样品离子色谱图中检测和鉴定了六种农药化合物。它们包括氯氰菊酯、乙酰甲胺磷、氯氟氰菊酯、氟氯菊酯、毒死蜱和氯芬膦。农药污染的流行率被确定为样本量的54.5%。在已鉴定的农药残留中,50%是基于拟除虫菊酯类的化合物,另外50%是基于有机磷的化合物。六种已鉴定的杀虫剂中有四种是氯化化合物。开发、验证了一种快速、简单、廉价、有效、坚固、安全的基于铜(II)螯合反应的紫外-可见双光束分光光度法技术,该技术可产生有色的铜-农药络合物,并用于量化和比较卡塔叶样品中所选农药化合物的水平。对与铜(II)离子螯合的农药化合物进行的紫外-可见波长扫描测量显示,氯氰菊酯和乙酰甲胺磷的最大吸收分别在321和207nm处。根据UV-Vis定量技术开发的标准品校准曲线显示,氯氰菊酯和乙酰甲胺磷标准品在0.5-10.0µg/L(R2=0.99)的浓度范围内具有良好的线性。定量限估计值分别为0.25-0.26µg/L。所选样品(其中确认存在残留物)的UV-Vis定量结果显示,乙酰甲胺磷(一种有机磷残留物)的浓度水平(范围为2.897-7.978µg/L)高于氯氰菊酯(2.145µg/L)。所选样本中定量分析的农药含量低于最大残留限量。危险系数(HQ)在0.247-0.797之间。
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