摘要
通过50%氯溴异氰尿酸可湿性粉剂在烟草上的农药残留消解试验,探讨氯溴异氰尿酸在烟草上的合理使用准则。采用高效液相色谱法对烟草及土壤中氯溴异氰尿酸进行残留量分析。样品采用乙腈提取,三氯甲烷和石油醚萃取净化,紫外检测器(UVD)测定,检测波长为200nm,流动相甲醇与冰乙酸水溶液(pH值为4.0)的体积比为5∶95。结果表明,氯溴异氰尿酸最低检出限为5.0×10-10g,在烟叶中的平均回收率为85.01%～91.92%,相对标准偏差为1.36%～6.09%;在土壤中的平均回收率为84.49%～92.44%,相对标准偏差为1.01%～5.29%。该方法操作简便,分离效果好,准确度和精密度均达到定量分析要求。
The paper is aimed to discuss a method for residue analysis of bromochlorocyanuric acid in the tobacco and the soil by using 50 percent bromochlorocyanuric acid through the residues of pesticides decomposition trial. The reason for doing so is that the acid WP in the tobacco may have noticeable effects on the prevention of tobacco leaves from the attack of any bacterial, fungal, virus diseases, and therefore it is meaningful to keep the safety production of tobacco and innovation of tobacco chemical pesticides. For this, we have analyzed the residues of bromochlorocyanuric acid in tobacco leaves and the soil by using high-performance liquid chromatography. The extraction process we used can be shown as follows： 1. Add 10.0 g samples of fresh tobacco leaves and 20.0 g samples of soil into the 250 mL flask and then add 20 mL of distilled water （pH adjusted with glacial acetic acid is about 4.0） to them; 2. Next, add 80mL of acetonitrile （80 mL of acetone were added into samples of soil） after slightly shaking of the flask filled with sufficient sample soak and then extract it with a rotary oscillator for 1hour, with a process of filtration followed; 3. Collect 50 mL of filtrate and transferred into the 250 mL separated funnel. The purification process we have adopted can be shown as follows： 1. The above-mentioned extraction process can be done with 30 mL, 30 mL and 20 mL of chloroform added respectively and then the chloroform extraction phase was discarded; 2. And, then, extract the remaining water content with the petroleum ether and, then, discard it in the extraction phase, in which the extracted content can be collected and transferred into the 150mL flat-bottomed flask and let it evaporate to 2-3 mL in a rotary evaporator and then dilute it with methanol and Glacial acetic acid aqueous solution（pH 4.0）（5： 96, v/v） to volume of 5.0 mL; 3. Afterwards, bring 2 mL solution into the process, which is let through a film of 0.45 um. Using UV detector at 200 nm, the liquid phase was methanol/acetic acid aqueous solution （5： 95, v/v）. The analysis results of our tests show that the detection limit 5.0＆times;10-10 g under the condition of our method, in which the recovery ratio of Bromochlorocyanuric Acid in the tobacco was 85.01%-91.92% and the relative standard deviations were 1.36%-6.09%, whereas the recovery ratio of Bromochlorocyanuric Acid in the soil was 84.49%-92.44%, with the relative standard deviation being 1.01%-5.29%. From what is said above, it can be concluded that the method, though simple, can bring about nice separation effects, for its precision and accuracy can meet the demands of quantitative analysis.
出处
《安全与环境学报》
CAS
CSCD
北大核心
2012年第5期127-130,共4页
Journal of Safety and Environment
关键词
环境科学技术其他学科
烟草
土壤
氯溴异氰尿酸
高效液相色谱
残留分析
other disciplines of environmental science and technology
tobacco
soil
bromochlorocyanuric acid
high performance liquid chromatography
residue analysis
