本文選題：巴比妥類 + 苯并二氮卓類��； 參考：《沈陽藥科大學》2002年碩士論文

【摘要】： 常見的催眠安定劑有巴比妥類，苯并二氮卓類和吩噻嗪類藥物。由于這些藥物使用廣泛，比較容易獲得，因此自殺、他殺、服用過量等原因引起的中毒、致死案件時有發(fā)生，是目前司法鑒定中常見的藥物。對于該類藥物的分析檢測，目前主要采用液液萃取普通紫外光譜測定法，液液萃取分離法操作繁瑣、費溶劑、藥物萃取率低，，雜質(zhì)去除不徹底。固相萃取是70年代以來在液相色譜原理基礎(chǔ)上發(fā)展起來的具有操作簡便快速、萃取率高等優(yōu)點的分離提取方法。這一技術(shù)避免了液液萃取的不足，堪稱分離技術(shù)的一次革命。紫外導數(shù)光譜法是70年代以來在紫外光譜法基礎(chǔ)上發(fā)展起來的具有操作簡便快速、能有效消除雜質(zhì)干擾、靈敏度較高等優(yōu)點的檢測方法。固相萃取、紫外導數(shù)光譜法國內(nèi)研究尚少。本論文的研究目的是將兩種方法相結(jié)合，建立起一種藥物萃取率高、雜質(zhì)去除徹底，可適合安眠藥物中毒、致死案件檢驗、以操作簡便快速為主要特點的分析方法。 1 巴比妥藥物固相萃取——紫外差示導數(shù)光譜檢測法 本文建立了血、尿、肝、腎、肺、腦中巴比妥、苯巴比妥、戊巴比妥、異戊巴比妥、速可眠的分析方法。血、尿用水稀釋，臟器用6％高氯酸沉淀蛋白后，加0.4mLGDX_(301)樹脂振搖，濾集樹脂于小層析柱中，用 水 10mL淋洗，二氯甲烷洗脫，收集洗脫液 smL，揮干后用 0．45mol／L的 氫氧化鈉溶液4刀mL溶解剩余物，將所得溶液2等份，分別再加 2刀mL 0．45mol／L氫氧化鈉和 2．omL 0石mol／L氯化鉀一硼酸緩沖溶液制成 pH14 及pH10的溶液，以pH10的溶液為參比，測定pH14溶液的二階導數(shù)光 譜圖。檢出限：血、尿 1．3～2石 u g／mL，臟器 0．8～3．6 u g哈。革取率： 對于血、尿檢材除巳比妥革取率為68．83～69．94％以外，其余藥物革取率 均在95．8～98．5％范圍內(nèi)：臟器檢材除巴比妥茬取率為60刀2～67．32％以 外，其余藥物革取率均在83二～gi二％范圍內(nèi)。線性范圍：0．5～5 p g／。L。 二 苯并二氮卓類藥物固相葷取一紫外導數(shù)光譜檢測法 本文建立了血、尿、肝、腎、肺、腦中硝西伴、地西伴、去甲西伴。 替馬西伴、奧沙西伴、氟西拌和利眠寧的分析方法。血、尿用水稀釋， 臟器用6％高氯酸沉淀蛋白后，加0衛(wèi)dGDX301樹脂振搖，濾集樹脂于 小層析柱中，用水 10InL淋洗，二氯甲烷洗脫，收集洗脫液 smL，揮干 后用 0．lmol／L的鹽酸溶液 4，omL溶解剩余物，以 0．lmol／L的鹽酸溶液為 參比，測定二階導數(shù)光譜圖。檢出限：血、尿0．3～l二ovg／mL，臟器0石～ 2．46fig／g。革取率：血、尿檢材中7種藥物革取率均在83．l～101j％范圍 內(nèi)：臟器檢材中除利眠寧革取率為66．32～科刀3％，其余6種藥物舉取率 均在73．72～86．2％范圍內(nèi)。線性范圍：0。5～5 v g／mL。 3 吩暖嚎類藥物固相葷取一紫外導數(shù)光譜檢測法 本文建立了氯丙嚎、異丙像 三氟拉嚎、奮乃靜、氟奮乃靜及其代 謝物的分析方法。 2 血采用親水性固相材料硅藻土葷�。喝�1刀InL檢血，對于氯丙嚎和 其代謝產(chǎn)物氯丙噴亞礬用州 的緩沖溶液1．omL稀釋；對于異丙咦和其 代謝產(chǎn)物異丙嗓亞礬用pH12的緩沖溶液1．omL稀釋；對于三氟拉噴和其 代謝產(chǎn)物三氟拉噴亞礬用pH10的緩沖溶液1．omL稀釋；對于氟奮乃靜和 其代謝產(chǎn)物氟奮乃靜亞礬用 pH 10的緩沖溶液 1刀mL稀釋；對于奮乃靜用 pH7的緩沖溶液 1刀mL稀釋；對于奮乃靜的代謝產(chǎn)物奮乃靜亞硯用 pH 的緩沖溶液1．omL稀釋。加人裝有2．sg硅藻土的小層析柱中，用乙醚洗 脫（奮乃靜亞礬用二氯甲烷洗脫），收集洗脫液SInL，揮干。 尿、臟器采用親脂性固相材料GDX301＄取，臟器加乙臘沉淀蛋白， 加 25rnL 0．11。l／L氫氧化鈉溶液；尿用水稀釋后，加入 GDX3010石mL， 搖動 smin，濾集樹脂于小層析柱中，用 10InL水淋洗樹脂，用 H氯甲烷 洗脫藥物，收集洗脫液smL于干燥的小燒杯中，揮干。剩余物用0刀smoUL 硫酸4刀mL溶解，加入鋅粉0．ig，沸水浴加熱3min，放冷，測定＝階導 數(shù)光譜圖。檢出限：血 1．0～2刀 n g／mL，尿 07～1．3 u g／mL，臟器 0．9～ 2．3pg／g。摹取率：血83．7～97．7％，尿88＊～95．1％，臟器72．63～90．6％。 線性范圍：0．5～svg／InL。 4 分析方法的實際應(yīng)用 采用本文建立的方法對8只家兔分別灌服苯巴比妥、戊巴比妥、速 可眠、地西拌、硝西伴、氯丙嗡 異丙噴，不同時間處死，采取血、尿、 3 肝、腎、肺、腦檢材進行測定。結(jié)果（經(jīng)氣相色譜符核）8只家兔血、尿、 肝、腎、肺、腦檢材中含量見表1。 表l 瞰販巴比共麥、苯弄Lk卓是、嶺嚷味美菇物 家兔在種拾材巋物合號測定桔粵 兔號兔重 灌服藥物 藥量處死時間 測值（u分ml or u旮g） （kg）（g）…）血 尿 肝 腎 肺 腦 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

【學位授予單位】：沈陽藥科大學
【學位級別】：碩士
【學位授予年份】：2002
【分類號】：D919

【參考文獻】

相關(guān)期刊論文 前2條

1 譚家鎰,姜兆林,吳維蓉;固相萃取-紫外差示導數(shù)光譜法測定臟器組織中巴比妥類藥物含量[J];中國法醫(yī)學雜志;1995年03期

2 趙爾剛，張桂華，王洪林;一階導數(shù)光譜法測定唾液、餌料及血液中殺鼠迷的含量[J];中國食品衛(wèi)生雜志;1995年03期

本文編號：1889128