离子液体分散液相微萃

发布时间：2018-04-23 01:25

  本文选题：溴敌隆 + 分散液相微萃取　； 参考：《河南科技大学》2012年硕士论文

【摘要】：背景与目的溴敌隆（Bromadiolone），属第二代香豆素类抗凝血杀鼠剂，因其灭鼠效果好、对人畜毒性低，近年来在我国得到认同并普遍使用。但由于使用管理不当，造成了该类鼠药中毒、甚至死亡事件的增加。因此，建立快速高效的生物样品中溴敌隆的检测方法十分必要。 样品前处理是法医毒物分析的关键步骤，直接影响毒物的检出率。传统的样品前处理方法如固相萃取、液液萃取等，，存在操作繁琐费时、提取率低、需要使用大量对人体和环境有毒害作用的有机溶剂等问题。分散液相微萃取是由Rezaee等于2006年首次报道的一种新型样品前处理方法，该方法集采样、萃取和浓缩于一体，操作简便快速、成本低、富集效率高且环境友好，是一种很有应用前景的样品前处理技术。方法本研究将离子液体分散液相微萃取技术引入生物检材尿液和血浆中的溴敌隆前处理中，通过考察萃取剂和分散剂体积、样品pH、盐浓度、萃取时间和离心时间等因素，优化前处理条件，获得较好的前处理结果。采用HPLC对前处理样品进行检测。 结果选用离子液体1-己基-3-甲基咪唑六氟磷酸盐（[C_6MIM][PF_6]）为萃取剂，甲醇为分散剂，提取样品中的溴敌隆。优化后的溴敌隆分散液相微萃取操作条件为：萃取剂[C_6MIM][PF_6]50μL，分散剂甲醇100μL，样品溶液pH值5.0，萃取时间5min，离心时间8min。 本研究建立了溴敌隆的高效液相色谱分析方法。方法采用Symmetry C18反相柱分离，流动相由甲醇（A）、25mmol/L磷酸盐缓冲液（pH=3.0）（B）组成，等度洗脱，A+B=85+15（v/v），流量1.0mL/min，柱温30℃，检测波长260nm。溴敌隆在1.0~500.0μg/mL范围内线性关系良好，相对标准偏差（RSD）小于5%，方法灵敏度高、重现性佳。 在优化的实验条件下，尿液中溴敌隆的检出限为1.1ng/mL（S/N＞3），线性范围为0.01~5.0μg/mL，线性相关系数r=0.9997。空白样品中低、中、高浓度加标回收率分别为82.4%、93.0%、95.6%，相对标准偏差（n=6）分别为6.63%、3.89%、3.86%；血浆中检出限为1.1ng/mL（S/N＞3），线性范围为0.01~5.0μg/mL，线性相关系数r=0.9988。空白样品中低、中、高浓度加标回收率分别为76.4%、82.6%、92.1%，相对标准偏差（n=6）分别为4.17%、2.99%、1.67%。 结论方法可满足中毒样品分析的需要，已成功应用于尿液和血浆中溴敌隆的检测，取得了满意的结果。
[Abstract]:Background & objective Bromadioloneone, a kind of second generation coumarin anticoagulant rodenticide, has been recognized and widely used in China in recent years because of its good rodent killing effect and low toxicity to human and animal. However, due to improper management of the use of this type of rodent poisoning, and even increased the number of deaths. Therefore, it is necessary to establish a rapid and efficient method for the determination of bromodiolone in biological samples. Sample pretreatment is a key step in forensic toxicological analysis, which directly affects the detection rate of poison. Traditional sample pretreatment methods such as solid-phase extraction liquid-liquid extraction and so on have many problems such as tedious and time-consuming operation low extraction rate and the need to use a large number of organic solvents which have toxic effects on human body and environment. Dispersive liquid phase microextraction (DLME) is a new sample pretreatment method first reported by Rezaee in 2006. The method integrates sampling, extraction and concentration, and is simple and rapid, low cost, high enrichment efficiency and environmentally friendly. It is a promising sample pretreatment technology. Methods the ion liquid dispersive liquid phase microextraction technique was introduced into the pretreatment of bromadiolone in urine and plasma of biological samples. The factors such as the volume of extractant and dispersant, the pH of the sample, the concentration of salt, the extraction time and the centrifugation time were investigated. The preprocessing conditions were optimized to obtain better pretreatment results. The pretreated samples were detected by HPLC. Results Ionic liquid [C_6MIM] [PF_6] was used as extractant and methanol as dispersant to extract bromadiolone from the sample with ionic liquid 1-hexyl-3-methyl imidazole hexafluorophosphate ([C_6MIM] [PF_6]) as extractant. The optimized conditions were as follows: extraction agent [C_6MIM] [PF_6] 50 渭 L, dispersant methanol 100 渭 L, pH value of sample solution 5.0, extraction time 5 min and centrifugation time 8 min. A high performance liquid chromatography (HPLC) method for the determination of bromadiolone was established. Methods the mobile phase was separated by Symmetry C18 reversed phase column. The mobile phase consisted of methanolamine 25 mmol / L phosphate buffer (pH = 3. 0), isophoric elution, flow rate was 1.0 mL / min, column temperature was 30 鈩

本文编号：1789837