水和生物体液中曲马多镇痛药的中空纤维膜液—液微萃取
发布时间：2019-03-15 07:38
【摘要】： 前言 曲马多是一种非吗啡类镇痛药物，长期服用会成瘾，但至今仍未管制，社会上滥用现象严重。本次实验以较新的样品前处理技术——中空纤维膜液相微萃取(HF-LPME)，对含有曲马多的水和生物检材进行检验。LPME是LLE的微型化，，污染少，成本低，方便，快速，萃取浓缩一步完成。 材料和方法 惠普HP-5890气相色谱仪；FID检测器；Easy3000色谱工作站；熔融石英毛细管柱HP-1(甲基硅酮)，膜厚0.52μm，内径0.32mm，长25m；温控磁力搅拌器：中空纤维膜；盐酸曲马多由市售药片经结晶与重结晶精制而成，经熔点测定符合药典要求；杜冷丁内标物由公安部物证鉴定中心提供；血浆和尿样采于健康人；有机溶剂甲苯、异辛烷、环己烷与氯仿。 首先，分别找到曲马多和杜冷丁的色谱峰位置和保留时间；其次，制作中空纤维膜液相微萃取装置；再次，设定原始萃取条件；第四，对萃取条件进行优化，方法为单变法；第五，在最佳的条件下萃取；最后，统计、分析结果，得出结论。 实验结果 曲马多和杜冷丁在设定的色谱条件之下得到了较好的分离，表现在峰形、分离度和保留时间。自来水、尿和血浆中的标准曲线回归方程分别为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(血浆)。实测结果表明最低检测限可达0.01μg／ml(自来和尿)和0.05μg／ml(血浆)。1ug／ml浓度的RSD达到5.15(水)、4.03(尿)、16.64(血浆)。 结论 HF-LPME是一种新颖、有效、简单、绿色环保的样品前处理技术，和其他前处理技术相比，具有以下特点：1、萃取溶剂的选择范围宽，因此可以提高萃取的选择性；2、萃取装置简单、成本低；3、简便、快速、易于对微小量的样品提取，使用萃取溶剂的量极少；4、可手工操作，亦可实现自动化。事实证明，LPME将萃取溶剂减小到了极限，是液液萃取方法的微型化，也是传统萃取方法的有力补充。本实验中，我们应用这种发法成功地萃取并用GC分析了滥用药物曲马多。本方法在法医毒物分析中的应用前景好。 本文尝试使用新技术，建立了从生物样品中提取曲马多的简便快速的方法。在室温(20℃)下用聚偏氟乙烯中空纤维膜过滤提取15min，仅使用4μl有机溶剂。曲马多作为一种非管制类的镇痛药物，它的滥用现状值得社会关注，而对于曲马多的检测也是当今具有实际意义的科学问题。而本实验中建立的方法作为传统方法的补充将会被更多实验室认可和应用。
[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
本文编号：2440427
[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
本文编号：2440427
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