CN102507793A - Method for detecting poison quickly by using blood - Google Patents
Method for detecting poison quickly by using blood Download PDFInfo
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- CN102507793A CN102507793A CN2011103787706A CN201110378770A CN102507793A CN 102507793 A CN102507793 A CN 102507793A CN 2011103787706 A CN2011103787706 A CN 2011103787706A CN 201110378770 A CN201110378770 A CN 201110378770A CN 102507793 A CN102507793 A CN 102507793A
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Abstract
The invention discloses a method for detecting poison quickly by using blood. The method comprises the following steps of: taking two pieces of blood to be detected; diluting one piece of blood by adding a pH9 buffer solution and diluting the other piece of blood by adding water; pouring the two pieces of blood into chromatographic columns with diatomite respectively; eluting the blood diluted with the pH9 buffer solution by using ether after passing through the chromatographic column, and concentrating the elution in a water bath at the temperature of 45 DEG C to obtain an extract A; eluting the blood diluted with the water by using dichloromethane after passing through the chromatographic column, and concentrating the elution in a water bath at the temperature of 50 DEG C and draining to obtain an extract B; and detecting the extract A and the extract B by using a detecting instrument for the conventional compounds respectively so as to detect the poison. According to the invention, a diatomite quick detection method applicable to the poisons (nearly covering all the poisons) is established; two samples are required, extraction is finished within 5 minutes for detection, and impurities are removed completely; and therefore detection time of the poisons is shortened and the detection operation is greatly simplified.
Description
Technical field
The invention belongs to the compound test field, specifically, relate to a kind of adopt blood carry out fast detecting in the method for which kind of poisonous substance.
Background technology
The analytical control of blood 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.
China is main tradition, the classical LLE liquid liquid extraction of adopting before the nineties in 20th century, and this method exists complex operation, expense solvent, extract drugs rate low, poor reproducibility, and Impurity removal is not thorough, is prone to shortcomings such as emulsification.Phase early 1990s; China's lipophilicity solid phase material (is main with GDX) method for distilling that begins one's study; This technology has been avoided a lot of deficiencies of liquid-liquid extraction, and extraction ratio obviously improves, but still has complex operation, time-consuming problems such as (the blood examination material extract generally and needs 120 minutes).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 blood, 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 blood fast detecting institute toxicity; Its key is: get two parts of blood to be checked; Portion adds the dilution of pH9 damping fluid, and another part thin up is poured into respectively and is equipped with in the diatomaceous chromatographic column; Use the ether wash-out after the blood that adds pH9 damping fluid dilution is crossed zeyssatite chromatography post, eluent concentrates dried to the greatest extent extract A in 40～45 ℃ water-bath; The blood of thin up is used the methylene chloride wash-out after crossing zeyssatite chromatography post; Eluent in 50～55 ℃ water-bath concentrate do to the greatest extent extract B; Utilize the detecting instrument of the compound that routinizes to detect respectively extract A and extract B, can detect and be which kind of poisonous substance.
Concrete grammar is: the blood to be checked of getting two parts of each 1.0mL; Portion adds pH9 damping fluid 1.0mL dilution; Another part adds water 1.0mL dilution; Pour into respectively and be equipped with in the diatomaceous chromatographic column of 2.3g, use the ether wash-out after the blood that adds pH9 damping fluid dilution is crossed chromatographic column, collect the 6mL eluent and concentrate in 45 ℃ water-bath and use up the dried extract A that obtains; The blood of thin up is used the methylene chloride wash-out after crossing chromatographic column, collects the 6mL eluent in the concentrated dried extract B that obtains to the greatest extent of 50 ℃ water-bath, utilizes the detecting instrument of the compound that routinizes to detect respectively extract A and extract B, can detect to be which kind of poisonous substance.
The detecting instrument of the said compound that routinizes is gas chromatograph-mass spectrometer (GCMS) and liquid chromatograph-mass spectrometer.Though the solution after the extraction can adopt instruments such as gas chromatography, high performance liquid chromatography, ultraviolet spectrometer (UVS) to detect, these instruments are not suitable for the screening analysis of unknown poisonous substance, drugs, medicine.Utilize the gas chromatograph-mass spectrometer (GCMS) Equipment Inspection more practical, quick.
Extracting data sees shown in the table 1.
Table 12-1: following ether of the different pH values of each medicine and methylene chloride wash-out zeyssatite extraction method extraction ratio in the blood
※Experiment is not done in "-" expression in the table
As can be seen from the table, after two samples are all crossed diatomite chromatography post, adopt no dilution and eluent, can realize basically can both detecting effective extraction of institute's Toxic.
Beneficial effect: the present invention has set up in the blood barbiturates medicine, Benzodiazepines medicine, the phenothiazines 10 types of zeyssatite method for quick that (having covered all basically) poisonous substance all is suitable for such as medicine, common drugs, alkaloid, the chronic rat poison of indandione class, the chronic rat poison of Hydroxycoumarin class, Tetramine acute rodenticide, organophosphorus insecticides, carbamate insecticides of sleeping peacefully of sleeping peacefully of sleeping peacefully; Only need two samples; Accomplish in 5 minutes to extract and detect, it is thorough to remove impurity.Can detect rapidly and be which kind of poisonous substance, shorten detection time, the operation of detection has been simplified greatly.
Embodiment
Embodiment
Get the blood to be checked of two parts of each 1.0mL; Portion adds pH9 damping fluid 1.0mL dilution; Another part adds water 1.0mL dilution; Pour into respectively 2.3g be housed! the real back of Dun 8mL) in the diatomaceous chromatographic column, after crossing chromatographic column, the blood that adds the dilution of pH9 damping fluid use the ether wash-out, and collect the 6mL eluent and concentrate the most dried extract A that obtains in 40～45 ℃ water-bath; The blood of thin up is used the methylene chloride wash-out after crossing chromatographic column; Collect the 6mL eluent in the concentrated dried extract B that obtains to the greatest extent of 50～55 ℃ water-bath; Utilize the detecting instrument (gas chromatograph-mass spectrometer (GCMS) and liquid chromatograph-mass spectrometer) of the compound that routinizes to detect respectively extract A and extract B then, can detect and be which kind of poisonous substance.
Claims (3)
1. method that adopts blood fast detecting institute toxicity; It is characterized in that: get two parts of blood to be checked; Portion adds the dilution of pH9 damping fluid, and another part thin up is poured into respectively and is equipped with in the diatomaceous chromatographic column; Use the ether wash-out after the blood that adds pH9 damping fluid dilution is crossed zeyssatite chromatography post, eluent concentrates dried to the greatest extent extract A in 40～45 ℃ water-bath; The blood of thin up is used the methylene chloride wash-out after crossing zeyssatite chromatography post; Eluent in 50～55 ℃ water-bath concentrate do to the greatest extent extract B; Utilize the detecting instrument of the compound that routinizes to detect respectively extract A and extract B, can detect and be which kind of poisonous substance.
2. according to the said a kind of method that adopts blood fast detecting institute toxicity of claim 1; It is characterized in that: the blood to be checked of getting two parts of each 1.0mL; Portion adds pH9 damping fluid 1.0mL dilution, and another part adds water 1.0mL dilution, pours into respectively and is equipped with in the diatomaceous chromatographic column of 2.3g; Use the ether wash-out after the blood that adds pH9 damping fluid dilution is crossed chromatographic column, collect the 6mL eluent and concentrate in 45 ℃ water-bath and use up the dried extract A that obtains; The blood of thin up is used the methylene chloride wash-out after crossing chromatographic column, collects the 6mL eluent in the concentrated dried extract B that obtains to the greatest extent of 50 ℃ water-bath, utilizes the detecting instrument of the compound that routinizes to detect respectively extract A and extract B, can detect to be which kind of poisonous substance.
3. according to claim 1 or 2 said a kind of methods that adopt blood fast detecting institute toxicity, it is characterized in that: the detecting instrument of the said compound that routinizes is gas chromatograph-mass spectrometer (GCMS) and liquid chromatograph-mass spectrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103787706A CN102507793A (en) | 2011-11-24 | 2011-11-24 | Method for detecting poison quickly by using blood |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103787706A CN102507793A (en) | 2011-11-24 | 2011-11-24 | Method for detecting poison quickly by using blood |
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| CN102507793A true CN102507793A (en) | 2012-06-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203674A (en) * | 2015-10-26 | 2015-12-30 | 吴玉红 | Rapid screening and extraction method of unknown medicines and toxins in samples |
| CN105388058A (en) * | 2015-10-26 | 2016-03-09 | 吴玉红 | Method for simultaneously and quickly extracting multi-target drugs and toxicants in detected material |
| CN107192788A (en) * | 2017-05-10 | 2017-09-22 | 山东省公安厅 | The gaschromatographic mass spectrometry screening method of unknown poisonous substance in blood |
| CN108133794A (en) * | 2018-02-13 | 2018-06-08 | 上海市刑事科学技术研究院 | The detection application of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine * * class drugs |
-
2011
- 2011-11-24 CN CN2011103787706A patent/CN102507793A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 吴玉红: "硅藻土提取紫外导数光谱法测定血中马钱子碱", 《辽宁警专学报》 * |
| 吴玉红等: "硅藻土固相萃取在毒物分析中的应用", 《中国人民公安大学学报(自然科学版)》 * |
| 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》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203674A (en) * | 2015-10-26 | 2015-12-30 | 吴玉红 | Rapid screening and extraction method of unknown medicines and toxins in samples |
| CN105388058A (en) * | 2015-10-26 | 2016-03-09 | 吴玉红 | Method for simultaneously and quickly extracting multi-target drugs and toxicants in detected material |
| CN107192788A (en) * | 2017-05-10 | 2017-09-22 | 山东省公安厅 | The gaschromatographic mass spectrometry screening method of unknown poisonous substance in blood |
| CN108133794A (en) * | 2018-02-13 | 2018-06-08 | 上海市刑事科学技术研究院 | The detection application of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine * * class drugs |
| CN108133794B (en) * | 2018-02-13 | 2019-08-02 | 上海市刑事科学技术研究院 | The detection application of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine * * class drug |
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Application publication date: 20120620 |