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固相萃取—气相色谱法测定香蕉中的有机磷农药

2014-08-11李春赵东兴李芹王树明

热带农业科学 2014年2期
关键词:固相萃取

李春++赵东兴++李芹++王树明

摘 要 为建立固相萃取-气相色谱法测定香蕉中多种残留有机磷农药敌敌畏、乐果、毒死蜱、辛硫磷、丙溴磷的方法,采用氮磷检测器(NPD)气相色谱法对经无水丙酮提取、Na2SO4脱水、固相萃取净化、氮吹仪浓缩后,用丙酮定容的样品进行测定。结果显示,敌敌畏、乐果、毒死蜱、辛硫磷、丙溴磷的最低检出浓度分别为0.010、0.008、0.012、0.002、0.008 mg/kg,加标回收率在78.82%~101.5%,相对标准偏差为3.7%~6.2%。表明该方法线性良好,回收率、精密度好,灵敏度高,符合检测要求,可用于香蕉中多种残留有机磷农药的测定。

关键词 固相萃取 ;气相色谱法 ;有机磷农药 ;香蕉

分类号 TQ450.7

Determination of Organophosphorous Pesticide in Bananas by Solid Phase Extraction Coupled with Gas Chromatography

LI Chun ZHAO Dongxing LI Qin WANG Shuming

(Honghe Institute of Tropical Agricultural Sciences of Yunnan, Hekou, Yunnan 661300)

Abstract In order to establish a method for determination of organophosphorous pesticide in bananas by solid phase extraction (SPE) coupled with gas chromatography (GC). Dichlorvos, daphene, chlorpyrifos, phoxim and profenofos were selected as the analytic targets organophosphorous pesticide. The result was determined by nitrogen-phosphorus (NPD) detector after acetone extraction, dehydrated by anhydrous sodium sulfate, solid phase extraction (SPE) purification, concentrated by Nitrogen blowing instrument and dissolved to constant volume with acetone. The limits of detection of these pesticide were 0.010, 0.008, 0.012, 0.002 and 0.008 mg/kg, respectively. The recoveries varied between 78.82% and 101.5%, and the relative standard deviations (RSD) was between 3.7% and 6.2%. The results shows that this method has reliable productivity and can give a good linear relationship with good recovery and RSD. So it is suitable for the analysis of organophosphorous pesticide in bananas.

Keywords solid phase extraction ; gas chromatography ; organophosphorous pesticide ; banana

香蕉(Musa nana Lour.)是热带、南亚热带地区的主要经济作物之一,然而在香蕉生产过程中会遭受多种病虫害的危害,为了保障香蕉的产量和质量,蕉农会使用大量的化学农药,从而使香蕉中的农药残留问题成为人们关注的焦点。

有机磷农药(OPS)作为一类高效、广谱的杀虫剂被用于香蕉的病虫害防治。但有机磷农药毒性很大,甚至有剧毒,其残留通过食物链,会出现一次性急性反应或在人体内积累而致畸、致癌、致突变[1]。因此,有必要建立一种能快速准确检测香蕉中有机磷农药的分析方法。

目前对蔬菜水果中有机磷农药的检测方法主要是通过固相萃取对样品净化后,采用气相色谱法[2-4]、气相色谱-质谱联用法[5-6]、免疫分析[7]、液相色谱-质谱联用法[8]进行分析。香蕉是一种高糖高胶质的水果,要求在提取时样品要得到较好的分散,现有的报道中只见到单一的有机磷农药在香蕉中的检测[9-10],尚未见到同时检测香蕉中的几种有机磷农药的报道。……

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