【摘要】： 前言 曲馬多是一種非嗎啡類鎮(zhèn)痛藥物，長(zhǎng)期服用會(huì)成癮，但至今仍未管制，社會(huì)上濫用現(xiàn)象嚴(yán)重。本次實(shí)驗(yàn)以較新的樣品前處理技術(shù)——中空纖維膜液相微萃取(HF-LPME)，對(duì)含有曲馬多的水和生物檢材進(jìn)行檢驗(yàn)。LPME是LLE的微型化，，污染少，成本低，方便，快速，萃取濃縮一步完成。 材料和方法 惠普HP-5890氣相色譜儀；FID檢測(cè)器；Easy3000色譜工作站；熔融石英毛細(xì)管柱HP-1(甲基硅酮)，膜厚0.52μm，內(nèi)徑0.32mm，長(zhǎng)25m；溫控磁力攪拌器：中空纖維膜；鹽酸曲馬多由市售藥片經(jīng)結(jié)晶與重結(jié)晶精制而成，經(jīng)熔點(diǎn)測(cè)定符合藥典要求；杜冷丁內(nèi)標(biāo)物由公安部物證鑒定中心提供；血漿和尿樣采于健康人；有機(jī)溶劑甲苯、異辛烷、環(huán)己烷與氯仿。 首先，分別找到曲馬多和杜冷丁的色譜峰位置和保留時(shí)間；其次，制作中空纖維膜液相微萃取裝置；再次，設(shè)定原始萃取條件；第四，對(duì)萃取條件進(jìn)行優(yōu)化，方法為單變法；第五，在最佳的條件下萃取；最后，統(tǒng)計(jì)、分析結(jié)果，得出結(jié)論。 實(shí)驗(yàn)結(jié)果 曲馬多和杜冷丁在設(shè)定的色譜條件之下得到了較好的分離，表現(xiàn)在峰形、分離度和保留時(shí)間。自來水、尿和血漿中的標(biāo)準(zhǔn)曲線回歸方程分別為Y=0.721X+0.0411，r~2=0.9997(水)；Y=0.587X+0.0564，r~2=0.9948(尿)；Y=1.0041X+0.0301，r~2=0.9985(血漿)。實(shí)測(cè)結(jié)果表明最低檢測(cè)限可達(dá)0.01μg／ml(自來和尿)和0.05μg／ml(血漿)。1ug／ml濃度的RSD達(dá)到5.15(水)、4.03(尿)、16.64(血漿)。 結(jié)論 HF-LPME是一種新穎、有效、簡(jiǎn)單、綠色環(huán)保的樣品前處理技術(shù)，和其他前處理技術(shù)相比，具有以下特點(diǎn)：1、萃取溶劑的選擇范圍寬，因此可以提高萃取的選擇性；2、萃取裝置簡(jiǎn)單、成本低；3、簡(jiǎn)便、快速、易于對(duì)微小量的樣品提取，使用萃取溶劑的量極少；4、可手工操作，亦可實(shí)現(xiàn)自動(dòng)化。事實(shí)證明，LPME將萃取溶劑減小到了極限，是液液萃取方法的微型化，也是傳統(tǒng)萃取方法的有力補(bǔ)充。本實(shí)驗(yàn)中，我們應(yīng)用這種發(fā)法成功地萃取并用GC分析了濫用藥物曲馬多。本方法在法醫(yī)毒物分析中的應(yīng)用前景好。 本文嘗試使用新技術(shù)，建立了從生物樣品中提取曲馬多的簡(jiǎn)便快速的方法。在室溫(20℃)下用聚偏氟乙烯中空纖維膜過濾提取15min，僅使用4μl有機(jī)溶劑。曲馬多作為一種非管制類的鎮(zhèn)痛藥物，它的濫用現(xiàn)狀值得社會(huì)關(guān)注，而對(duì)于曲馬多的檢測(cè)也是當(dāng)今具有實(shí)際意義的科學(xué)問題。而本實(shí)驗(yàn)中建立的方法作為傳統(tǒng)方法的補(bǔ)充將會(huì)被更多實(shí)驗(yàn)室認(rèn)可和應(yīng)用。
[Abstract]:Tramadol is a kind of non-morphine analgesic drug. Long-term use of tramadol may become addictive, but it is still unregulated, and the abuse in society is serious. In this experiment, hollow fiber membrane liquid phase microextraction (HF-LPME), a new sample pretreatment technique, was used to examine water and biological samples containing tramadol. LPME is a miniaturization of LLE with low pollution, low cost, convenience and rapidity. The extraction and concentration is completed in one step. Materials and methods Hewlett-Packard HP-5890 gas chromatography; FID detector; Easy3000 chromatograph workstation; fused silica capillary column HP-1 (methylsilicone), film thickness 0.52 渭 m, inner diameter 0.32mm, length 25m; Temperature-controlled magnetic agitator: hollow fiber membrane; tramadol hydrochloride is refined by crystallization and recrystallization and met the requirements of Pharmacopoeia by melting point determination; the internal standard of Dulengding is provided by the material identification center of the Ministry of Public Security; Plasma and urine samples were taken from healthy people; organic solvents toluene, isooctane, cyclohexane and chloroform. Firstly, the position of chromatographic peak and retention time of tramadol and Dulengding were found respectively; secondly, the liquid phase microextraction device of hollow fiber membrane was made; thirdly, the original extraction conditions were set; fourth, the extraction conditions were optimized by univariate method; Fifth, under the optimal conditions, extraction; finally, statistics, analysis of the results, draw a conclusion. The results showed that tramadol and Dulengding were separated well under the set chromatographic conditions, which showed peak shape, separation degree and retention time. The regression equations of standard curve in tap water, urine and plasma were Y = 0.721X 0.0411, r = 2 = 0.9997 (water), Y = 0.587x 0.0564 (r = 0.0564), r = 0.9948 (urine), Y = 1.0041x 0.0301 (P < 0.01), r = 2 = 0.9985 (plasma), respectively. The results showed that the minimum detection limits were 0.01ug / ml and 0.05ug / ml respectively. The RSD of 1ug / ml was 5.15 (water), 4.03 (urine) and 16.64 (plasma). Conclusion HF-LPME is a novel, effective, simple and environmentally friendly sample pretreatment technique. Compared with other pretreatment techniques, it has the following characteristics: 1. The selection range of extraction solvent is wide. Therefore, the selectivity of extraction can be improved. 2, the extraction device is simple, low cost; 3, simple, rapid, easy to extract small amount of sample, the amount of solvent extraction is very small; 4, can be operated by hand, but also can be automated. It has been proved that LPME reduces the extraction solvent to the limit, which is not only the miniaturization of liquid-liquid extraction method, but also a powerful supplement to the traditional extraction method. In this experiment, we successfully extracted and analyzed tramadol by GC. The application prospect of this method in forensic toxicological analysis is good. A simple and rapid method for extracting tramadol from biological samples was established by using a new technique. At room temperature (20 鈩

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