Department for Medicines Quality Control, Institute for Public Health of the Republic of Macedonia, Skopje, Republic of Macedonia.
J Environ Sci Health B. 2010 Oct;45(7):694-701. doi: 10.1080/03601234.2010.502462.
An isocratic High Performance Liquid Chromatographic (HPLC) method was optimized for 3-phenoxybenzyl (1RS)-cis-trans-3-(2,2-dichlorovinyl)-2,2-dimethyl-cyclopropanecarboxylate (permethrin) residues identification and quantification in wine matrix. Analytical reverse phase (RP) C-18 column was used (25 cm × 4 mm i.d., 5 μ m) with mobile phase consisting of acetonitrile and water in ratio 70 %/30 % (v v(-1)), flow-rate 2.0 mL min(-1), UV-detection at 215 nm and controlled oven temperature at 25°C. The peaks of isomers were identified with the retention times as compared to standard cis-/trans- mixture and confirmed with characteristic spectra using photodiode array detector. Under these conditions, permethrin isomers were well separated with resolution 2.8 and no interference with the naturally present wine compounds was observed. The method was validated for linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). Linear regression analysis data proved a good linear relationship (correlation coefficients, r(2), for cis- and trans-isomer are: 0.9995 and 0.9997, respectively) between response of the detector and concentration of permethrin isomers over a wide concentration range for both isomers (0.55 mg L(-1) -4.40 mg L(-1)). Experimental data showed mean recoveries between 93.95% and 96.58% with RSD values in range: 0.89% -3.69%. The effect of ethanol content in the solvent on permethrin isomers peak areas was also studied and 60% v v(-1) ethanol was found to be optimal for sample preparation. The method was successfully tested on 20 commercial wine samples from the market in which no permethrin was detected. Thus, it was proved that it is suitable for routine permethrin residues analysis. The proposed method is suitable for routine analysis because of the simple sample preparation, acceptable run-time, low cost and its applicability with conventional instruments.
建立了一种高效液相色谱法(HPLC),用于 3-苯氧苄基(1RS)-顺式-反式-3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷羧酸酯(氯菊酯)在葡萄酒基质中的残留分析和定量检测。采用反相(RP)C18 柱(25cm×4mm i.d.,5μm),流动相为乙腈和水,体积比为 70%/30%(v/v),流速为 2.0mL min-1,在 215nm 处进行紫外检测,柱温为 25℃。通过与标准顺式/反式混合物的保留时间比较,对异构体的峰进行了鉴定,并使用光电二极管阵列检测器对特征光谱进行了确认。在这些条件下,氯菊酯异构体得到了很好的分离,分辨率为 2.8,并且没有观察到与天然存在的葡萄酒化合物的干扰。该方法对线性、精密度、准确度、检测限(LOD)和定量限(LOQ)进行了验证。线性回归分析数据表明,顺式和反式异构体的检测器响应与氯菊酯异构体浓度之间存在良好的线性关系(相关系数 r2 分别为 0.9995 和 0.9997),两种异构体的浓度范围均很宽(0.55mgL-1-4.40mgL-1)。实验数据表明,两种异构体的平均回收率在 93.95%至 96.58%之间,相对标准偏差(RSD)值在 0.89%至 3.69%之间。还研究了溶剂中乙醇含量对氯菊酯异构体峰面积的影响,发现 60%v/v 的乙醇最适合样品制备。该方法成功地应用于 20 个市售葡萄酒样品的检测,未检出氯菊酯。因此,证明该方法适用于常规氯菊酯残留分析。该方法简单、运行时间短、成本低、适用于常规仪器,因此适用于常规分析。