固相萃

发布时间：2018-05-14 19:15

本文选题：巴比妥类 + 苯并二氮卓类　；参考：《沈阳药科大学》2002年硕士论文

【摘要】： 常见的催眠安定剂有巴比妥类，苯并二氮卓类和吩噻嗪类药物。由于这些药物使用广泛，比较容易获得，因此自杀、他杀、服用过量等原因引起的中毒、致死案件时有发生，是目前司法鉴定中常见的药物。对于该类药物的分析检测，目前主要采用液液萃取普通紫外光谱测定法，液液萃取分离法操作繁琐、费溶剂、药物萃取率低，，杂质去除不彻底。固相萃取是70年代以来在液相色谱原理基础上发展起来的具有操作简便快速、萃取率高等优点的分离提取方法。这一技术避免了液液萃取的不足，堪称分离技术的一次革命。紫外导数光谱法是70年代以来在紫外光谱法基础上发展起来的具有操作简便快速、能有效消除杂质干扰、灵敏度较高等优点的检测方法。固相萃取、紫外导数光谱法国内研究尚少。本论文的研究目的是将两种方法相结合，建立起一种药物萃取率高、杂质去除彻底，可适合安眠药物中毒、致死案件检验、以操作简便快速为主要特点的分析方法。 1 巴比妥药物固相萃取——紫外差示导数光谱检测法本文建立了血、尿、肝、肾、肺、脑中巴比妥、苯巴比妥、戊巴比妥、异戊巴比妥、速可眠的分析方法。血、尿用水稀释，脏器用6％高氯酸沉淀蛋白后，加0.4mLGDX_(301)树脂振摇，滤集树脂于小层析柱中，用水 10mL淋洗，二氯甲烷洗脱，收集洗脱液 smL，挥干后用 0．45mol／L的氢氧化钠溶液4刀mL溶解剩余物，将所得溶液2等份，分别再加 2刀mL 0．45mol／L氢氧化钠和 2．omL 0石mol／L氯化钾一硼酸缓冲溶液制成 pH14 及pH10的溶液，以pH10的溶液为参比，测定pH14溶液的二阶导数光谱图。检出限：血、尿 1．3～2石 u g／mL，脏器 0．8～3．6 u g哈。革取率：对于血、尿检材除巳比妥革取率为68．83～69．94％以外，其余药物革取率均在95．8～98．5％范围内：脏器检材除巴比妥茬取率为60刀2～67．32％以外，其余药物革取率均在83二～gi二％范围内。线性范围：0．5～5 p g／。L。二苯并二氮卓类药物固相荤取一紫外导数光谱检测法本文建立了血、尿、肝、肾、肺、脑中硝西伴、地西伴、去甲西伴。替马西伴、奥沙西伴、氟西拌和利眠宁的分析方法。血、尿用水稀释，脏器用6％高氯酸沉淀蛋白后，加0卫dGDX301树脂振摇，滤集树脂于小层析柱中，用水 10InL淋洗，二氯甲烷洗脱，收集洗脱液 smL，挥干后用 0．lmol／L的盐酸溶液 4，omL溶解剩余物，以 0．lmol／L的盐酸溶液为参比，测定二阶导数光谱图。检出限：血、尿0．3～l二ovg／mL，脏器0石～ 2．46fig／g。革取率：血、尿检材中7种药物革取率均在83．l～101j％范围内：脏器检材中除利眠宁革取率为66．32～科刀3％，其余6种药物举取率均在73．72～86．2％范围内。线性范围：0。5～5 v g／mL。 3 吩暖嚎类药物固相荤取一紫外导数光谱检测法本文建立了氯丙嚎、异丙像三氟拉嚎、奋乃静、氟奋乃静及其代谢物的分析方法。 2 血采用亲水性固相材料硅藻土荤取：取1刀InL检血，对于氯丙嚎和其代谢产物氯丙喷亚矾用州的缓冲溶液1．omL稀释；对于异丙咦和其代谢产物异丙嗓亚矾用pH12的缓冲溶液1．omL稀释；对于三氟拉喷和其代谢产物三氟拉喷亚矾用pH10的缓冲溶液1．omL稀释；对于氟奋乃静和其代谢产物氟奋乃静亚矾用 pH 10的缓冲溶液 1刀mL稀释；对于奋乃静用 pH7的缓冲溶液 1刀mL稀释；对于奋乃静的代谢产物奋乃静亚砚用 pH 的缓冲溶液1．omL稀释。加人装有2．sg硅藻土的小层析柱中，用乙醚洗脱（奋乃静亚矾用二氯甲烷洗脱），收集洗脱液SInL，挥干。尿、脏器采用亲脂性固相材料GDX301＄取，脏器加乙腊沉淀蛋白，加 25rnL 0．11。l／L氢氧化钠溶液；尿用水稀释后，加入 GDX3010石mL，摇动 smin，滤集树脂于小层析柱中，用 10InL水淋洗树脂，用 H氯甲烷洗脱药物，收集洗脱液smL于干燥的小烧杯中，挥干。剩余物用0刀smoUL 硫酸4刀mL溶解，加入锌粉0．ig，沸水浴加热3min，放冷，测定＝阶导数光谱图。检出限：血 1．0～2刀 n g／mL，尿 07～1．3 u g／mL，脏器 0．9～ 2．3pg／g。摹取率：血83．7～97．7％，尿88＊～95．1％，脏器72．63～90．6％。线性范围：0．5～svg／InL。 4 分析方法的实际应用采用本文建立的方法对8只家兔分别灌服苯巴比妥、戊巴比妥、速可眠、地西拌、硝西伴、氯丙嗡异丙喷，不同时间处死，采取血、尿、 3 肝、肾、肺、脑检材进行测定。结果（经气相色谱符核）8只家兔血、尿、肝、肾、肺、脑检材中含量见表1。表l 瞰贩巴比共麦、苯弄Lk卓是、岭嚷味美菇物家兔在种拾材岿物合号测定桔粤兔号兔重灌服药物药量处死时间测值（u分ml or u旮g）（kg）（g）…）血尿肝肾肺脑 12 苯巴比妥 05 2 1067 678 996 786 732 726 2 3 戊巴比妥 03 2
[Abstract]:Common hypnotic stabilizers are barbiturates, benzodiazoides and phenothiazines. Because these drugs are widely used, they are easy to obtain, so the cases of poisoning caused by suicide, homicide, overdose and so on are common in the judicial identification. The analysis and detection of this kind of drugs is currently the main method. Liquid liquid extraction is used for ordinary UV spectrophotometry. Liquid liquid extraction separation method is complicated, solvent, drug extraction and impurity removal. Solid phase extraction is a method of separation and extraction with advantages of easy operation and high extraction rate developed on the basis of liquid chromatography on the basis of liquid chromatography in 70s. The deficiency of liquid extraction is a revolution of separation technology. Ultraviolet derivative spectrometry is a detection method, which has been developed on the basis of ultraviolet spectroscopy since 70s, which has the advantages of simple operation, simple operation, effective elimination of impurity interference and high sensitivity. The domestic research on solid phase extraction and ultraviolet derivative spectroscopy is still few. The purpose is to combine the two methods to establish an analytical method with high extraction rate and thorough removal of impurities, which can be suitable for sleeping drug poisoning, test of fatal cases and simple and rapid operation.
1 barbiturate solid phase extraction UV Differential derivative spectrophotometry
A method of analysis of blood, urine, liver, kidney, lung, brain, barbiturate, phenobarbital, pentobarbital, isopentobarbital, and fast dormant was established. Blood, urine water was diluted, after the organs were precipitated with 6% perchloric acid, and 0.4mLGDX_ (301) resin was used to shake the resin in a small layer column.
Water 10mL was washed and dichloromethane was eluted, and eluent smL was collected. After drying, 0.45mol / L was used.
Sodium hydroxide solution 4 knives mL dissolved residues, the resulting solution 2 equal parts, then add two knife mL
0.45mol / L sodium hydroxide and 2.omL 0 stone mol / L potassium chloride boric acid buffer solution were made into pH14.
And the solution of pH10, with pH10 solution as reference, the two derivative light of pH14 solution is determined.
The limits of detection are: blood, urine 1.3 to 2 stone u g / mL, viscera 0.8 ~ 3.6 u g ha.
For blood and urine samples, except for the ratio of 68.83 to 69.94%, the rate of other leather leathers is higher.
They are all in the range of 95.8 to 98.5%: the rate of organ examination is 60 to 2 to 67.32% except barbiturates.
The yield of other leather medicines ranged from 83 to two GI 2%. The linear range was 0.5 to 5 p g /.L..
Determination of two benzo two azo drugs by solid phase extraction and derivative spectrophotometry
In this paper, blood, urine, liver, kidney, lung, brain, and the west side with the west side.
Method for analysis of the mixture of mmaxi, Osasi, fluoxi and lepronine.
The organ was precipitated with 6% perchloric acid, then added 0 dGDX301 resin to shake and filter the resin.
In the small column, 10InL was washed with water and dichloromethane was eluted, and the eluent smL was collected and dried.
Then use 0.lmol / L hydrochloric acid solution 4 and omL to dissolve the remainder and use 0.lmol / L hydrochloric acid as the solution.
For reference, the two order derivative spectrogram was determined. The detection limits were: blood, urine 0.3 ~ l two ovg / mL, viscera 0 stones.
2.46fig / g. leather extraction rate: blood, urine test materials in 7 kinds of leather leather extraction rates are in the range of 83.l to 101j%.
Internal: in the visceral examination, the rate of leather removal was 66.32 to 3%, and the remaining 6 drugs were selected.
They are all in the range of 73.72 to 86.2%. The linear range is 0.5 ~ 5 V g / mL..
Determination of 3 phenazone by solid phase ultraviolet spectrophotometry
In this paper, chlorpromazine, isoproterenol, three fluoroprophone, perphenazine, fluphenazine and its generation are established.
The analytical method of the metabolite.
Two
Blood was taken with hydrophilic solid phase diatomaceous soil: 1 knife InL blood was collected for chloropropane.
Its metabolite, chlorpromazine, is diluted with the buffer solution 1.omL of the state; for isopropyl and its
The metabolite isopropyl ammonium alum is diluted with pH12 buffer solution 1.omL; for three fluorine spray and its
The metabolite three fluorine spray alum was diluted with pH10 buffer solution 1.omL; for fluphenazine and
Its metabolite, fluphenazine alum, was diluted with pH 10 buffer solution 1 knife mL, for perphenazine.
PH7 buffer solution diluted with 1 knife mL; for perphenazine metabolite perphenazine inkstone with pH
The buffer solution was diluted with 1.omL. A small column containing 2.sg diatomite was washed with ether.
Remove (perphenazine) from dichloromethane and collect eluent SInL and dry.
Urine and viscera were taken from lipophilic solid phase GDX301, and the organs were added with precipitated protein.
Add 25rnL 0.11.l / L sodium hydroxide solution, dilute urine water and add GDX3010 stone mL.
Shake the smin, filter the resin in the small column, rinse the resin with 10InL water, and use H chloromethane.
The eluent was collected, and the eluent was collected in smL dry small beaker. The residue was dried with 0 knife smoUL.
Sulfuric acid 4 knives mL dissolved, add zinc powder 0.ig, boiling water bath heating 3min, cooling, determination = order.
Detection limits: blood 1 to 2 knife n g / mL, urine 07 to 1.3 u g / mL, viscera 0.9 ~
2.3pg / g. copy rate: Blood 83.7 to 97.7%, urine 88 ~ 95.1%, viscera 72.63 ~ 90.6%.
Linear range: 0.5 ~ SVG / InL.
The practical application of the 4 analysis method
The 8 rabbits were fed with phenobarbital, pentobarbital, and quickly.
Can sleep, West mixed, nitrite West, chlorpromazine, isopropyl, and kill at different times, take blood, urine,
Three
The liver, kidney, lung and brain samples were measured. Results (by gas chromatography) 8 rabbits had blood and urine.
Content of liver, kidney, lung, and brain, table 1.
Table l look at Barbie co Mai, benzen Lk Zhuo, Ling rang delicious mushrooms.
Determination of oranges and Cantonese in the rabbit with a pickled material
Rabbit rabbits were re administered with the dose of drugs (U ml or u g).
(kg) (g)... ) hematuria, liver and kidney, lung and brain
12 phenobarbital 052106767899678673 726
23 pentobarbital 032

【学位授予单位】：沈阳药科大学
【学位级别】：硕士
【学位授予年份】：2002
【分类号】：D919

【参考文献】