8%辛菌胺醋酸鹽水劑在煙草上的殘留分析及消解動態(tài)研究
本文選題:辛菌胺 + 煙草 ; 參考:《貴州大學(xué)》2016年碩士論文
【摘要】:本文運(yùn)用液相色譜三重串聯(lián)四級桿質(zhì)譜(LC-MS/MS),檢測辛菌胺在煙草中的殘留量。對辛菌胺在煙草上的消解動態(tài)和最終殘留進(jìn)行研究,為辛菌胺在煙草上安全使用和殘留檢測提供理論依據(jù)。土壤中的辛菌胺經(jīng)乙腈提取,取1 mL上清液,LC-MS/MS上機(jī)檢測。煙葉中的辛菌胺經(jīng)甲醇提取,取1 mL上清液,PSA和C18凈化,LC-MS/MS上機(jī)檢測。煙粉中的辛菌胺經(jīng)甲醇提取,取1 mL上清液,PSA和C18凈化,LC-MS/MS上機(jī)檢測。土壤中辛菌胺標(biāo)準(zhǔn)溶液的線性范圍為0.005~0.5μg/mL,煙葉中為0.005~0.5μg/mL,煙粉中為0.005~0.5μg/mL,相關(guān)性系數(shù)分別為0.9999、0.9999和1.0000。辛菌胺在土壤中的添加水平為0.01~1.0 mg/kg,回收率為81.24~107.5%,相對標(biāo)準(zhǔn)偏差(RSD)為1.19~6.75%;在煙葉中的添加水平為0.02~2.0 mg/kg,回收率為81.08~97.68%,相對標(biāo)準(zhǔn)偏差(RSD)為1.59~16.0%;在煙粉中的添加水平為0.05~5.0 mg/kg,回收率為97.93~103.9%,相對標(biāo)準(zhǔn)偏差(RSD)為3.30~8.80%。該方法均達(dá)到農(nóng)藥殘留檢測對于準(zhǔn)確度、精密度與靈敏度的要求。2014年和2015年分別在貴州省都勻市惠水縣擺金鎮(zhèn)、湖南省長沙市東岸鄉(xiāng)進(jìn)行了8%辛菌胺醋酸鹽水劑在煙草上的兩年兩地殘留試驗(yàn)研究,檢測土壤、煙葉和煙粉中的辛菌胺殘留量。結(jié)果表明:用藥量750~1125 g/ha,施藥3~4次,煙草移栽期用藥,收獲期采樣,2014和2015年收獲期煙草中辛菌胺的殘留量為0.05~0.71 mg/kg,殘留量中值為0.08 mg/kg。本文首次研究了不同環(huán)境條件下辛菌胺在土壤中的降解行為,探討其影響因素及其降解規(guī)律。結(jié)果表明:辛菌胺在土壤中藥劑質(zhì)量減小、微生物增多、有機(jī)質(zhì)含量高、含水率高都使其在土壤中的降解速率加快;辛菌胺在貴州土壤中降解速率較慢,其降解半衰期為7.4 d,在廣西與山東土壤中降解的半衰期分別為7.0d和6.9 d。辛菌胺在土壤中的降解主要受藥劑質(zhì)量、含水率以及微生物含量的影響。
[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.
【學(xué)位授予單位】:貴州大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2016
【分類號】:S481.8;O657.63
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