8%辛菌胺醋酸盐水剂在烟草上的残留分析及消解动态研究

发布时间：2018-05-28 21:05

本文选题：辛菌胺 + 烟草　；参考：《贵州大学》2016年硕士论文

【摘要】：本文运用液相色谱三重串联四级杆质谱(LC-MS/MS),检测辛菌胺在烟草中的残留量。对辛菌胺在烟草上的消解动态和最终残留进行研究,为辛菌胺在烟草上安全使用和残留检测提供理论依据。土壤中的辛菌胺经乙腈提取,取1 mL上清液,LC-MS/MS上机检测。烟叶中的辛菌胺经甲醇提取,取1 mL上清液,PSA和C18净化,LC-MS/MS上机检测。烟粉中的辛菌胺经甲醇提取,取1 mL上清液,PSA和C18净化,LC-MS/MS上机检测。土壤中辛菌胺标准溶液的线性范围为0.005~0.5μg/mL,烟叶中为0.005~0.5μg/mL,烟粉中为0.005~0.5μg/mL,相关性系数分别为0.9999、0.9999和1.0000。辛菌胺在土壤中的添加水平为0.01~1.0 mg/kg,回收率为81.24~107.5%,相对标准偏差(RSD)为1.19~6.75%;在烟叶中的添加水平为0.02~2.0 mg/kg,回收率为81.08~97.68%,相对标准偏差(RSD)为1.59~16.0%;在烟粉中的添加水平为0.05~5.0 mg/kg,回收率为97.93~103.9%,相对标准偏差(RSD)为3.30~8.80%。该方法均达到农药残留检测对于准确度、精密度与灵敏度的要求。2014年和2015年分别在贵州省都匀市惠水县摆金镇、湖南省长沙市东岸乡进行了8%辛菌胺醋酸盐水剂在烟草上的两年两地残留试验研究,检测土壤、烟叶和烟粉中的辛菌胺残留量。结果表明:用药量750~1125 g/ha,施药3~4次,烟草移栽期用药,收获期采样,2014和2015年收获期烟草中辛菌胺的残留量为0.05~0.71 mg/kg,残留量中值为0.08 mg/kg。本文首次研究了不同环境条件下辛菌胺在土壤中的降解行为,探讨其影响因素及其降解规律。结果表明:辛菌胺在土壤中药剂质量减小、微生物增多、有机质含量高、含水率高都使其在土壤中的降解速率加快;辛菌胺在贵州土壤中降解速率较慢,其降解半衰期为7.4 d,在广西与山东土壤中降解的半衰期分别为7.0d和6.9 d。辛菌胺在土壤中的降解主要受药剂质量、含水率以及微生物含量的影响。
[Abstract]:In this paper, the residue of octylamine in tobacco was determined by liquid chromatographic triple tandem quadruple mass spectrometry (LC-MS / MS). In order to provide a theoretical basis for the safe use and residual detection of octyl amine in tobacco, the dynamics and final residues of octyl amine in tobacco were studied. The soil was extracted by acetonitrile and 1 mL supernatant was detected by LC-MS / MS. The octyl amines in tobacco leaves were extracted by methanol, and 1 mL supernatant PSA and C18 purified by LC-MS / MS were used to detect. The octyl amines in tobacco powder were extracted by methanol, then 1 mL supernatant PSA and C18 purified by LC-MS / MS were detected. The linear range of standard solution of octamine in soil was 0.005 ~ 0. 5 渭 g / mL, in tobacco leaf was 0.005 ~ 0. 5 渭 g / mL, in tobacco powder was 0. 005 ~ 0. 5 渭 g / mL, the correlation coefficients were 0. 9999 and 1. 0000, respectively. The addition level of octamine in soil was 0.01g / kg, the recovery rate was 81.24mg / kg, the relative standard deviation (RSDs) was 1.19mg / kg, the addition level in tobacco was 0.02n 2.0 mg / kg, the recovery was 81.08mg / kg, the relative standard deviation (RSD) was 1.59mg / kg, and the addition level in tobacco powder was 0.05mg / kg, and the recovery was 0.05.0mgg. kg. The relative standard deviation (RSDs) was 97.93 / 103.9 and 3.30 / 8.80, respectively. The method meets the requirements of accuracy, precision and sensitivity for pesticide residue detection. In 2014 and 2015, the method was used in Zhujin Town, Huishui County, Duyun City, Guizhou Province, respectively. In Dongan Township, Changsha, Hunan Province, the residue of 8% octyllamine acetate in tobacco was studied for two years, and the residues of octylamine in soil, tobacco leaf and tobacco powder were detected. The results showed that the amount of drug was 750 ~ 1125g / ha, the dosage of 3 times was 3 times, the amount of octamine in tobacco was 0.050.71 mg / kg, the mean value was 0.08 mg 路kg ~ (-1) in the harvest period in 2014 and 2015, and the mean value was 0.08 mg 路kg ~ (-1) in tobacco during the transplanting period, and in the harvest period of 2014 and 2015, the residual amount of octamine in tobacco was 0.050.71 mg / kg. In this paper, the degradation behavior of octyl amines in soil under different environmental conditions was studied for the first time, and its influencing factors and degradation rules were discussed. The results showed that the degradation rate of octyl amine in Guizhou soil was slower than that in Guizhou soil, but the degradation rate of octyllamine was decreased, microorganism increased, organic matter content was high, moisture content was high, and the degradation rate of octyllamine in Guizhou soil was lower than that in Guizhou soil. The degradation half-life was 7.4 days, and the degradation half-life in Guangxi and Shandong soils was 7.0 and 6.9 days, respectively. The degradation of octyl amine in soil was mainly affected by the chemical quality, moisture content and microbial content.
【学位授予单位】：贵州大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：S481.8;O657.63

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