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烟草中有机氯农药残留标准测定方法的改进

Improvement of Standard Method for Determination of Organochlorine Pesticide Residue in Tobacco

  • 摘要: 为提高烟草中有机氯农药残留的检测种类和速度,对ISO 4389:2000(GB/T 13596-2004)法进行了改进。即用50%(体积分数)正己烷和50%(体积分数)丙酮混合溶剂代替正己烷作萃取剂,用加速溶卉4萃取代替索氏萃取.对萃取温度进行了优化,并采用改进法和ISO 4389:2000法分别检测了国内外65个烟草样品中有机氯农药残留。结果表明:①该法检出10个样品中残留β-硫丹,而GB/T 13596-2004法未检出;②除β-硫丹外,两种方法检出烟草样品中的有机氯农药的种类几乎一样,且测定量之间的差异符合痕量农药测定的变异系数在20%以下的要求;③17个烟叶样品中未检出任何有机氯农药,占所选烟叶样品数的26.2%,其它样品都或多或少地残留有机氯农药;④o,p'-DDT的检出率最高,达到43.1%,所有样品中均未检出狄氏剂和异狄氏剂;⑤国内外卷烟样品中检出的残留的有机氯农药种类分别为47个和43个。其中,进口卷烟中均检出了有机氧农药,且主要为α-硫丹、β-硫丹和o,p'-DDT,而国产卷烟中主要在4个样品中检出了这些农药;⑥国产烟叶样品中残留的有机氯农药种类比进口样品稍多,且都主要是由某些样品中检出,其它样品中残留的有机氯农药的种类较少;⑦所有检测样品中有机氯农药的残留量均低于CORESTA推荐限量。该法萃取自动化程度高,萃取时间(25 min)短,可替代ISO 4389:2000法进行烟草样品中有机氯农药残留的快速检测。

     

    Abstract: In order to increase the detectable number and test speed of organochlorine pesticide residue in tobacco, the standard method for determination of organochlorine pesticide residue in tobacco from ISO 4389:2000(GB/T 13596-2004) was improved. Soxhlet extraction and n-hexane (extracting solvent) were replaced by accelerated solvent extraction (ASE) and component solvent of w-hexane and acetone (1:1, v/v) f respectively, and extracting temperature was optimized. The residues of organochlorine pesticides in 65 domestic and imported tobacco samples were determined with the improved method and ISO 4389:2000 method, the results showed that:1) β -endosulfan was detected in 10 samples by the improved method, but not found by ISO 4389:2000; 2) the organochlorine pesticides detectable by both methods were almost the same except for β-endosulfan, quantitatively, their coefficients of variation were below the acceptable limits for trace pesticide determination of 20%; 3) no organochlorine pesticide was detectable in 17 samples t which accounted for 26.2% of total samples; 4) the detection rate of o, p' -DDT was the highest (up to 43. 1%), neither Dieldrin nor Endrin was detected in all samples;5) the numbers of detectable organochlorine pesticides were 47 and 43 in domestic and imported cigarette samples, respectively; organochlorine pesticides were detected in all of the imported samples, particularly α-endosulfan, β-endosulfan, and o, p'一DDT,while these pesti-cides were detectable only in 4 domestic samples; 6) the numbers of detectable pesticides in domestic leafsamples were slightly higher than that in imported samples, which happened mainly in a couple of domestic samples; 7) the residues of organochlorine pesticides in all samples were lower than CORESTA recommendedlimits. The improved method could replace ISO 4389:2000 in fast detection of the residues of organochlorinepesticides in tobacco samples.

     

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