摘要
为了确定鳊肌肉中乐果、甲基对硫磷、马拉硫磷3种有机磷农药GPC（凝胶渗透色谱）的最佳净化条件,运用＂完全随机设计2因素析因设计＂编辑不同的GPC单浓缩方法,通过气相色谱仪测定浓缩后农药溶液的浓度。比较样品浓度的标准偏差来确定GPC和气相色谱的精密度。比较有机磷农药加标回收率,用SPSS 16.0统计软件中的广义线性模型进行方差分析,确定适宜浓缩条件。通过持续分段收集法确定有机磷农药的适宜收集时间。采用确定的适宜收集时间和单浓缩条件对鳊肌肉中提取的有机磷农药进行净化。结果表明,在0.01~1.0 mg/L范围内3种农药组分含量与峰面积呈线性相关（相关系数为0.997~0.998）。乐果、甲基对硫磷、马拉硫磷的定性检出限分别为7.27 ng/kg、7.15 ng/kg、7.15 ng/kg,定量检出限分别为40.3 ng/kg、37.3 ng/kg、38.0 ng/kg。GPC净化的适宜条件：以环己烷∶乙酸乙酯=1∶1（体积比）为溶剂;柱流速为5.0 m L/min;定量进样环进样量为5.0 m L;除杂质时间为1 080 s,收集目标物时间为480s,洗柱时间为300 s;浓缩温度为40℃;第1阶段真空泵压力为18 000Pa或19 000 Pa,第2阶段真空泵压力为20 000 Pa或21 000 Pa。适宜净化条件下乐果、甲基对硫磷、马拉硫磷的回收率为83.59%~95.19%。在气相色谱仪和GPC精密度较好、标准工作曲线良好的情况下,确定了GPC对鳊肌肉中3种有机磷农药的适宜净化条件,回收率较好,检出限低于国家标准,符合淡水鱼类中有机磷农药的检测要求。
This paper is aimed at selecting the optimal purifying condition for the organophosphorus pesticides（ dimethoate,parathion-methyl,malathion） in the muscle of Parabramis pekinensis by means of gel permeation chromatography（ GPC）. For this purpose,we have worked out different GPC independent concentration methods by using the totally random＂2 ×2 factorial design＂and tested the concentration of the enriched solution with the gas chromatograph（ GC）. Furthermore,we have determined the precision of GPC and GC by testing the standard deviation of the sample concentration. Comparing the spiked recovery of the 3 kinds of organophosphorus pesticides and making the variance analysis by a general linear model of SPSS 16. 0,it is possible eventually to determine the optimal concentration condition. And,then,the optimal collection time for the organophosphorus pesticides with continuous sub-collection method can be determined. The organophosphorus pesticides in the muscle of Parabramis pekinensis can be purified under the condition of optimal collection time and independent concentration. The results of our research show that the contents of the 3 kinds of organophosphorus pesticides are by nature linearly related to the peak area in the range of 0. 01-1. 0 mg / L,whereas the correlation coefficients have been found equal to 0. 997- 0. 998,with the qualitative detection limits of method being 7. 27 ng / kg for dimethoate,7. 15 ng / kg for parathion-methyl,7. 15 ng / kg for malathion. Besides,the quantitative detection limits of the method are likely to be equal to 40. 3ng / kg for dimethoate,37. 3 ng / kg for parathion-methyl,and 38. 0 ng / kg for malathion. What is more,the optimum purification conditions of GPC prove to be： the volume ratio of cyclohexane to ethylacetate is 1∶ 1; the column flowing rate is 5. 0 m L/ min; the quantitative sample loop is 5. 0m L; the forerum time is 1 080 s,the main fraction time should be 480 s;the tailing time is 300 s; the concentration temperature is 40 ℃; the vacuum pump pressure at the first stage should be 18 000 Pa or 19 000 Pa,whereas the vacuum pump pressure at the second stage should be 20 000 Pa or 21 000 Pa. Under such optimum purification condition,the recovering rates of dimethoate,parathion-methyl and malathion should be found from 83. 59% to 95. 19%,respectively. In the case of fine precision of the GC,GPC standard curves,the optimal purifying conditions of organophosphorus pesticides in the muscle of Parabramis pekinensis by GPC can be determined with the spiked recovering rate being fine below the national standard. The results have thus can be thought to come in accord with the testing demands of the organophosphorus pesticide in the freshwater fishery culturing criteria.
出处
《安全与环境学报》
CAS
CSCD
北大核心
2015年第3期279-284,共6页
Journal of Safety and Environment
基金
浙江省分析测试计划项目(2012C37064)
关键词
环境工程学
GPC
净化
鳊肌肉
有机磷
气相色谱
environmental engineering
GPC
purification
Parabramis pekinensis
organophosphorus
GC
