生物样品中百草枯和呋喃丹的分析研究
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摘要
随着生活水平的不断提高，人们对健康的关注越来越多。特别是农产品的安全问题被提到很高的关注程度。但是，近年来，由于农药污染食品、饮水污染或自服、误服引起的中毒却还是屡见不鲜。本文以高效液相色谱为手段，以生物材料做为研究对象，研究了生物样品中的农药百草枯和呋喃丹。论文主要包括以下内容：
研究了百草枯的测定体系，通过对百草枯分光光度法的实验总结，建立了快速检测百草枯离子的快速检测方法，百草枯离子在0.5-10μg·mL~(-1)浓度范围内呈良好的线性关系，线性回归曲线为：y=0.01548+0.22109x，相关系数r=0.99985。通过对前处理的研究、流动相的选择、离子对试剂的选择、pH的影响、流动相添加剂的浓度等方面的研究，确定在流动相为9∶1的水：乙腈中添加了5mmol·L~(-1)庚烷磺酸钠和40mmol·L~(-1)三乙胺，并且调整流动相pH为3.0的情况下，应用UV-VIS检测器，在254nm处对生物样品尿中的百草枯的测定进行了研究。百草枯在100ng·mL~(-1)—500μg·mL~(-1)浓度范围内与检测器响应信号成良好的线性关系(r=0.99974)。建立了一种以反相离子对色谱法检测百草枯的方法。此方法具有快速、灵敏度高、定量准确、结果稳定的优点，可用于尿中百草枯浓度的监测。
研究了呋喃丹的测定体系，通过对前处理方法的研究、流动相选择、流速、以及温度等方面的研究，确定了各种因素对反相高效液相色谱测定生物样品中呋喃丹的影响，确定了在流动相为甲醇∶水为1∶1，流速在1.0mL·min~(-1)，温度35℃的条件下，样品经乙腈除蛋白的情况下，应用UV-VIS检测器，在280nm处对尿中的呋喃丹进行的研究。呋喃丹在0.2μg·mL~(-1)—10μg·mL~(-1)浓度范围内线性关系良好(r=0.99915)。该方法经济实用，可以用于24小时以内尿中呋喃丹浓度的监测。
Along with the living level raising continuously, people are more and more concerned over the health of themselves.Especially the safe of agricultural product is spoken of very high concern level.But, in recent years, it is not very fresh to see poisoning affairs because of polluted food, polluted water taken or miss taken pesticide.In this study, high performance liquid chromatography instrument is used to detect pesticide residue in biological samples . The thesis mainly includes following contents:
Investigations had been performed on the determination of paraquat. After many times experimentation, developed a new fast method to analyze paraquat in urine by Spectrophotometry. Paraquat at a concentration range of 0.5-10μg/mL in urine were determined with high accuracy and precision The relationship of the peak current and the paraquart was y=0.01548+0.22109x, (r=0.99985). In study of the effect of the pre-treated method, the mobile phase, ion-pair reagent, the pH, and other additive stauff .At last we chose water and acetonitrile at 9: 1 as the mobile phase, added 1-Heptanesulfonic acid (5mmol·L~(-1)) and triethylamine(40mmol·L~(-1)). pH was adjusted to 3. The relationship of the peak current and the paraquat concentration was in the range of 100ng·mL~(-1)—500μg·mL~(-1) (r=0.99974). The detection limits of paraquat was 25ng·mL~(-1), the recovery was 88.28%-95.47%. The method had been applied to the determination of paraquat in urine satisfactory result.
Investigations had been performed on the pre-treated method , the mobile phase, , the pH, the temperature and other stauff. The urine was pre-treaed by acetonitrile.The mobile phase was water and methanol at 1:1 The flow rate was 1.0mL/min, and the temperature at 35℃. The UV-VIS detector wavelengh was adjusted to 280nm. The relationship of the peak current and the paraquat concentration was in the range of 0.2μg/mL—10μg/mL(r=0.999l5). This metod was very economy, it could be used to inspect the concentration of carbofuran in urine.
研究了百草枯的测定体系，通过对百草枯分光光度法的实验总结，建立了快速检测百草枯离子的快速检测方法，百草枯离子在0.5-10μg·mL~(-1)浓度范围内呈良好的线性关系，线性回归曲线为：y=0.01548+0.22109x，相关系数r=0.99985。通过对前处理的研究、流动相的选择、离子对试剂的选择、pH的影响、流动相添加剂的浓度等方面的研究，确定在流动相为9∶1的水：乙腈中添加了5mmol·L~(-1)庚烷磺酸钠和40mmol·L~(-1)三乙胺，并且调整流动相pH为3.0的情况下，应用UV-VIS检测器，在254nm处对生物样品尿中的百草枯的测定进行了研究。百草枯在100ng·mL~(-1)—500μg·mL~(-1)浓度范围内与检测器响应信号成良好的线性关系(r=0.99974)。建立了一种以反相离子对色谱法检测百草枯的方法。此方法具有快速、灵敏度高、定量准确、结果稳定的优点，可用于尿中百草枯浓度的监测。
研究了呋喃丹的测定体系，通过对前处理方法的研究、流动相选择、流速、以及温度等方面的研究，确定了各种因素对反相高效液相色谱测定生物样品中呋喃丹的影响，确定了在流动相为甲醇∶水为1∶1，流速在1.0mL·min~(-1)，温度35℃的条件下，样品经乙腈除蛋白的情况下，应用UV-VIS检测器，在280nm处对尿中的呋喃丹进行的研究。呋喃丹在0.2μg·mL~(-1)—10μg·mL~(-1)浓度范围内线性关系良好(r=0.99915)。该方法经济实用，可以用于24小时以内尿中呋喃丹浓度的监测。
Along with the living level raising continuously, people are more and more concerned over the health of themselves.Especially the safe of agricultural product is spoken of very high concern level.But, in recent years, it is not very fresh to see poisoning affairs because of polluted food, polluted water taken or miss taken pesticide.In this study, high performance liquid chromatography instrument is used to detect pesticide residue in biological samples . The thesis mainly includes following contents:
Investigations had been performed on the determination of paraquat. After many times experimentation, developed a new fast method to analyze paraquat in urine by Spectrophotometry. Paraquat at a concentration range of 0.5-10μg/mL in urine were determined with high accuracy and precision The relationship of the peak current and the paraquart was y=0.01548+0.22109x, (r=0.99985). In study of the effect of the pre-treated method, the mobile phase, ion-pair reagent, the pH, and other additive stauff .At last we chose water and acetonitrile at 9: 1 as the mobile phase, added 1-Heptanesulfonic acid (5mmol·L~(-1)) and triethylamine(40mmol·L~(-1)). pH was adjusted to 3. The relationship of the peak current and the paraquat concentration was in the range of 100ng·mL~(-1)—500μg·mL~(-1) (r=0.99974). The detection limits of paraquat was 25ng·mL~(-1), the recovery was 88.28%-95.47%. The method had been applied to the determination of paraquat in urine satisfactory result.
Investigations had been performed on the pre-treated method , the mobile phase, , the pH, the temperature and other stauff. The urine was pre-treaed by acetonitrile.The mobile phase was water and methanol at 1:1 The flow rate was 1.0mL/min, and the temperature at 35℃. The UV-VIS detector wavelengh was adjusted to 280nm. The relationship of the peak current and the paraquat concentration was in the range of 0.2μg/mL—10μg/mL(r=0.999l5). This metod was very economy, it could be used to inspect the concentration of carbofuran in urine.
引文
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