CN102435690A - Method for quickly detecting poison in liver - Google Patents
Method for quickly detecting poison in liver Download PDFInfo
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- CN102435690A CN102435690A CN2011103787782A CN201110378778A CN102435690A CN 102435690 A CN102435690 A CN 102435690A CN 2011103787782 A CN2011103787782 A CN 2011103787782A CN 201110378778 A CN201110378778 A CN 201110378778A CN 102435690 A CN102435690 A CN 102435690A
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Abstract
The invention discloses a method for quickly detecting a poison in the liver, which comprises the following steps of: adding perchloric acid with mass concentration of 6% into liver sample homogenate, shaking out, centrifuging, and taking supernate at different times; adding 6% perchloric acid into the residuum, similarly operating, and merging the two kinds of supernate; dividing the supernate into two parts, wherein the PH of one part of the supernate is adjusted to be 9-12, the part of the supernate is poured into a chromatographic column filled with kieselguhr, and the other part of the supernate is directly poured into another chromatographic column filled with kieselguhr; eluting two parts of supernate by dichloromethane, collecting eluent, and completely concentrating at 50 DEG C water bath to obtain two parts of extractive; and detecting the extractive, so that the type of the poison can be detected. According to the invention a technology for performing perchloric acid release and kieselguhr solid phase material systematic extraction to medicine, poison and narcotics in the liver is established, the release and the extraction of the unknown medicine, poison and narcotics in the liver can be completed within 15 minutes, and the method is simple, convenient and fast, high in extraction ratio and thorough in impurity removal.
Description
Technical field
The invention belongs to the compound test field, specifically, relate to a kind of adopt liver carry out fast detecting in the method for which kind of poisonous substance.
Background technology
The analytical control of liver Chinese traditional medicine, poisonous substance, drugs is divided into extracts and detects two links.Because the progress of science and technology; The instrumental analysis detection technique has had significant progress; And extractive technique also is in developing stage, set up simple and convenient fast, extraction ratio is high, Impurity removal is thorough, can be fit to multiple medicine, system's method for distilling of poisonous substance, drugs analytical control seems particularly important.
The liver extractive technique was divided into for two steps, at first was the drug in the liver is come out, and the medicine that is about in the tissue enters into the WS abundantly---and this also is present domestic and international research difficult point.Second step was that the extract drugs in the WS is come out.
The method of having reported of carrying out drug release process homogenization is in a organized way got the supernatant method after adding the water mixing, is got supernatant method, acid-hydrolysis method, enzyme hydrolysis method etc. after adding the protein precipitant mixing.Enzyme hydrolysis method belongs to a kind of biochemical method, and enzyme preparation is difficult to be obtained, and enzyme activity is subject to influence such as condition of storage and is difficult to ensure that it is longer that enzymolysis takes time, and is easy inadequately quick, and WS complicated component, and impurity is more in the extract.Acid-hydrolysis method is simple than enzymatic isolation method; We had once carried out the extraction research of barbiturates medicine, phenothiazines medicine in the liver, and (the Benzodiazepines medicine is decomposes under acid condition; Be not suitable for this law), research shows, have the barbiturate acidolysis only after extraction ratio satisfied result is arranged; But detection limit is higher, and this method neither be first-selected.Tissue homogenateization is got the supernatant method after adding the water mixing, and drug release rate is low, and impurity is many.Tissue homogenateization is got the supernatant method after adding the protein precipitant mixing, and comparatively easy fast supernatant is as clear as crystal, and impurity is less, is method preferably.This method has bibliographical information, but all is to single medicine or single type of medicine.In practice, about five or six ten kinds of the poisonous substance in the most normal, the public security officer is in the detection process, and the poisonous substance of being met is these five or six ten kinds basically.At present, the method for distilling of being studied is general only to single or single type of medicine, as being directed against these five or six ten kinds of poisonous substances; Need to want several different methods to purify respectively, can all not adapt to, when detecting, just need to prepare a plurality of samples with a kind of method; The extraction of carrying out several different methods could cover institute's Toxic, and workload is very big, detects simultaneously to be the sort of poisonous substance; Need long time, can not realize fast detecting.
Summary of the invention
For solving above technical matters, the object of the present invention is to provide a kind of employing liver, the method for the fast detecting institute toxicity that the time is short, simple to operate.
The present invention seeks to realize like this: a kind of method that adopts liver fast detecting institute toxicity is characterized in that: get the perchloric acid that the liver sample homogenization adds mass concentration 6%, and jolting, centrifugal, obtain supernatant; Add 6% perchloric acid in the residue again, the same operation merges twice supernatant; Supernatant is divided into 2 parts, and wherein 1 part of accent pH is 9～12, pours into and is equipped with in the diatomaceous chromatographic column; In addition directly pour another into and be equipped with in the diatomaceous chromatographic column for 1 part; All use the methylene chloride wash-out, collect eluent, concentrate the dried to the greatest extent two parts of extracts that obtain in 50～55 ℃ of water-baths; Utilize the detecting instrument of the compound that routinizes to detect respectively two parts of extracts, can detect and be which kind of poisonous substance.
Get the perchloric acid 3.0mL that 1.0g liver sample homogenization adds mass concentration 6%, jolting, centrifugal, obtain supernatant; Add 6% perchloric acid 1.5mL in the residue again, the same operation merges twice supernatant; Supernatant is divided into 2 parts, and wherein 1 part of accent pH is 9～12, pours into and is equipped with in the diatomaceous chromatographic column of 3.0g; In addition directly pour another into and be equipped with in the diatomaceous chromatographic column of 3.0g for 1 part; All use the methylene chloride wash-out, collect the 6mL eluent, concentrate the dried to the greatest extent two parts of extracts that obtain in 50 ℃ of water-baths; Utilize the detecting instrument of the compound that routinizes to detect respectively two parts of extracts, can detect and be which kind of poisonous substance.
The detecting instrument of the above-mentioned compound that routinizes is gas chromatograph-mass spectrometer (GCMS) or liquid chromatograph-mass spectrometer.Though the solution after the extraction can adopt gas chromatography, high performance liquid chromatography, ultraviolet spectrometer (UVS) etc. to detect, these instruments are not suitable for unknown toxicological analysis.If adopt this Equipment Inspection of gas chromatograph-mass spectrometer (GCMS) more practical, quick.
Extracting data sees shown in the table 1.
Table 1 liver Chinese traditional medicine perchloric acid precipitation albumen zeyssatite extraction method extraction ratio
From table, can find out that two samples are all crossed zeyssatite chromatography post, before crossing post, adopt adjustment pH to realize effective extraction ratio of (having covered all basically poisonous substances).
Beneficial effect: we have set up the present invention and liver Chinese traditional medicine, poisonous substance, drugs have been carried out perchloric acid discharges and zeyssatite solid phase material system extractive technique; Can accomplish the release and the extraction of unknown medicine, poisonous substance, drugs in the liver in 15 minutes, simple and convenient fast, extraction ratio is high, Impurity removal is thorough.
Embodiment
Embodiment
Get the perchloric acid 3mL that 1.0g liver sample homogenization adds mass concentration 6%, jolting, centrifugal, obtain supernatant; Add 6% perchloric acid 1.5mL in the residue again, the same operation merges twice supernatant; Supernatant is divided into 2 parts, and wherein 1 part of accent pH is 9～12, pours into and is equipped with in the diatomaceous chromatographic column of 3.0g; In addition directly pour another into and be equipped with in the diatomaceous chromatographic column of 3.0g for 1 part; All use the methylene chloride wash-out, collect the 6mL eluent, concentrate the dried to the greatest extent two parts of extracts that obtain in 50～55 ℃ of water-baths; Utilize the detecting instrument (gas chromatograph-mass spectrometer (GCMS), liquid chromatograph-mass spectrometer) of the compound that routinizes to detect respectively two parts of extracts, can detect and be which kind of poisonous substance.
Claims (3)
1. method that adopts liver fast detecting institute toxicity is characterized in that: get the perchloric acid that the liver sample homogenization adds mass concentration 6%, and jolting, centrifugal, obtain supernatant; Add 6% perchloric acid in the residue again, the same operation merges twice supernatant; Supernatant is divided into 2 parts, and wherein 1 part of accent pH is 9～12, pours into and is equipped with in the diatomaceous chromatographic column; In addition directly pour another into and be equipped with in the diatomaceous chromatographic column for 1 part; All use the methylene chloride wash-out, collect eluent, concentrate the dried to the greatest extent two parts of extracts that obtain in 50～55 ℃ of water-baths; Utilize the detecting instrument of the compound that routinizes to detect respectively two parts of extracts, can detect and be which kind of poisonous substance.
2. according to the said a kind of method that adopts liver fast detecting institute toxicity of claim 1, it is characterized in that: get the perchloric acid 3.0mL that 1.0g liver sample homogenization adds mass concentration 6%, jolting, centrifugal, obtain supernatant; Add 6% perchloric acid 1.5mL in the residue again, the same operation merges twice supernatant; Supernatant is divided into 2 parts, and wherein 1 part of accent pH is 9～12, pours into and is equipped with in the diatomaceous chromatographic column of 3.0g; In addition directly pour another into and be equipped with in the diatomaceous chromatographic column of 3.0g for 1 part; All use the methylene chloride wash-out, collect the 6mL eluent, concentrate the dried to the greatest extent two parts of extracts that obtain in 50 ℃ of water-baths; Utilize the detecting instrument of the compound that routinizes to detect respectively two parts of extracts, can detect and be which kind of poisonous substance.
3. according to claim 1 or 2 said a kind of methods that adopt liver fast detecting institute toxicity, it is characterized in that: the detecting instrument of the said compound that routinizes is gas chromatograph-mass spectrometer (GCMS) or liquid chromatograph-mass spectrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103787782A CN102435690A (en) | 2011-11-24 | 2011-11-24 | Method for quickly detecting poison in liver |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103787782A CN102435690A (en) | 2011-11-24 | 2011-11-24 | Method for quickly detecting poison in liver |
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| CN102435690A true CN102435690A (en) | 2012-05-02 |
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| CN2011103787782A Pending CN102435690A (en) | 2011-11-24 | 2011-11-24 | Method for quickly detecting poison in liver |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104833743A (en) * | 2015-05-18 | 2015-08-12 | 公安部物证鉴定中心 | Method for analyzing cathinone, methcathinone and 4-methylmethcathinone in biological sample by liquid chromatography-mass spectrometry |
| CN106986834A (en) * | 2017-05-26 | 2017-07-28 | 山东新华制药股份有限公司 | The preparation method of 5 ethyl 5 (1 methyl butyl) barbiturates sodium |
-
2011
- 2011-11-24 CN CN2011103787782A patent/CN102435690A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 吴玉红等: "一种简便、快速测定肝脏中马钱子碱和士的宁含量的方法", 《第五次全国法医学术交流会论文集》 * |
| 吴玉红等: "肝中巴比妥类药物硅藻土固相提取法", 《辽宁大学学报》 * |
| 吴玉红等: "血尿肝中巴比妥类药物硅藻土提取紫外差示导数光谱测定", 《中国法医学杂志》 * |
| 吴玉红等: "血尿肝中毒鼠强硅藻土提取GC/NPD检测法", 《刑事技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104833743A (en) * | 2015-05-18 | 2015-08-12 | 公安部物证鉴定中心 | Method for analyzing cathinone, methcathinone and 4-methylmethcathinone in biological sample by liquid chromatography-mass spectrometry |
| CN106986834A (en) * | 2017-05-26 | 2017-07-28 | 山东新华制药股份有限公司 | The preparation method of 5 ethyl 5 (1 methyl butyl) barbiturates sodium |
| CN106986834B (en) * | 2017-05-26 | 2019-08-09 | 山东新华制药股份有限公司 | The preparation method of 5- ethyl -5- (1- methyl butyl) barbiturates sodium |
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Application publication date: 20120502 |