本文選題：溴敵隆 + 分散液相微萃取�。� 參考：《河南科技大學(xué)》2012年碩士論文

【摘要】：背景與目的溴敵�。˙romadiolone），屬第二代香豆素類抗凝血?dú)⑹髣蚱錅缡笮Ч�、�?duì)人畜毒性低，近年來(lái)在我國(guó)得到認(rèn)同并普遍使用。但由于使用管理不當(dāng)，造成了該類鼠藥中毒、甚至死亡事件的增加。因此，建立快速高效的生物樣品中溴敵隆的檢測(cè)方法十分必要。 樣品前處理是法醫(yī)毒物分析的關(guān)鍵步驟，直接影響毒物的檢出率。傳統(tǒng)的樣品前處理方法如固相萃取、液液萃取等，，存在操作繁瑣費(fèi)時(shí)、提取率低、需要使用大量對(duì)人體和環(huán)境有毒害作用的有機(jī)溶劑等問(wèn)題。分散液相微萃取是由Rezaee等于2006年首次報(bào)道的一種新型樣品前處理方法，該方法集采樣、萃取和濃縮于一體，操作簡(jiǎn)便快速、成本低、富集效率高且環(huán)境友好，是一種很有應(yīng)用前景的樣品前處理技術(shù)。方法本研究將離子液體分散液相微萃取技術(shù)引入生物檢材尿液和血漿中的溴敵隆前處理中，通過(guò)考察萃取劑和分散劑體積、樣品pH、鹽濃度、萃取時(shí)間和離心時(shí)間等因素，優(yōu)化前處理?xiàng)l件，獲得較好的前處理結(jié)果。采用HPLC對(duì)前處理樣品進(jìn)行檢測(cè)。 結(jié)果選用離子液體1-己基-3-甲基咪唑六氟磷酸鹽（[C_6MIM][PF_6]）為萃取劑，甲醇為分散劑，提取樣品中的溴敵隆。優(yōu)化后的溴敵隆分散液相微萃取操作條件為：萃取劑[C_6MIM][PF_6]50μL，分散劑甲醇100μL，樣品溶液pH值5.0，萃取時(shí)間5min，離心時(shí)間8min。 本研究建立了溴敵隆的高效液相色譜分析方法。方法采用Symmetry C18反相柱分離，流動(dòng)相由甲醇（A）、25mmol/L磷酸鹽緩沖液（pH=3.0）（B）組成，等度洗脫，A+B=85+15（v/v），流量1.0mL/min，柱溫30℃，檢測(cè)波長(zhǎng)260nm。溴敵隆在1.0~500.0μg/mL范圍內(nèi)線性關(guān)系良好，相對(duì)標(biāo)準(zhǔn)偏差（RSD）小于5%，方法靈敏度高、重現(xiàn)性佳。 在優(yōu)化的實(shí)驗(yàn)條件下，尿液中溴敵隆的檢出限為1.1ng/mL（S/N＞3），線性范圍為0.01~5.0μg/mL，線性相關(guān)系數(shù)r=0.9997。空白樣品中低、中、高濃度加標(biāo)回收率分別為82.4%、93.0%、95.6%，相對(duì)標(biāo)準(zhǔn)偏差（n=6）分別為6.63%、3.89%、3.86%；血漿中檢出限為1.1ng/mL（S/N＞3），線性范圍為0.01~5.0μg/mL，線性相關(guān)系數(shù)r=0.9988。空白樣品中低、中、高濃度加標(biāo)回收率分別為76.4%、82.6%、92.1%，相對(duì)標(biāo)準(zhǔn)偏差（n=6）分別為4.17%、2.99%、1.67%。 結(jié)論方法可滿足中毒樣品分析的需要，已成功應(yīng)用于尿液和血漿中溴敵隆的檢測(cè)，取得了滿意的結(jié)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

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