CN102590189B - Method for detecting and pretreating nitroglycerin solution nitrate - Google Patents
Method for detecting and pretreating nitroglycerin solution nitrate Download PDFInfo
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- CN102590189B CN102590189B CN201210022466.2A CN201210022466A CN102590189B CN 102590189 B CN102590189 B CN 102590189B CN 201210022466 A CN201210022466 A CN 201210022466A CN 102590189 B CN102590189 B CN 102590189B
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Abstract
The invention discloses a method for detecting and pretreating nitroglycerin solution nitrate. The method comprises the following steps: naturally volatilizing the solvent of the detected sample under the condition of room temperature and normal pressure or room temperature or reduced pressure; dissolving purified water by residues; vibrating; placing and laminating; filtering; and applying the filtrate to a nitrate brown ring test, wherein the junction cannot show brown at once. Compared with the prior art, the invention has the advantages that the technology fills the gap of the medicinal nitroglycerin solution nitrate detection technology; the condition of combustion or explosion of nitroglycerin caused by the conventional nitrate detection method is eliminated successfully; the method is high in accuracy and high in stability; and the method is particularly suitable for large-scale production detection operation.
Description
Technical field
The present invention relates to the inspection method of nitrate, detection and the pre-treating method thereof of nitrate in especially medicinal nitroglycerin solution.
Background technology
Nitroglycerin solution is the bulk drug of producing vasodilator agent nitroglycerin injection.At present, to refer generally to concentration be 10% monobel ethanol solution to the medicinal nitroglycerin solution of standard.
Monobel chemistry trinitin by name, colourless or yellow clarification oily liquids, is slightly soluble in water, is soluble in ethanol, ether, acetone.Be subject to sudden and violent cold sudden-heat, shock, friction, while meeting bright pry-, all have the danger setting off an explosion.Contact kickback can occur with strong acid, cause burning or blast.
To be glycerine do under the condition of nitrating agent quantitatively nitrated forming at nitric acid and sulfuric acid acid mixture with monobel, adopts a large amount of purified water wash-outs excessive nitric acid and sulfuric acid, but still have the nitrate of part residual in technological process.In the process of placing at nitroglycerin solution, also easily there is degraded and generation nitrate.In order to monitor better the quality of medicinal nitroglycerin solution, improve product purity, reduce the toxic and side effect of nitroglycerin injection, it is very necessary that wherein residual nitrate impurity is detected.
In the prior art, the detection method of nitrate has multiple, comprising brown ring test, HPLC method etc.For example, " Chinese Pharmacopoeia " two of versions in 2010 have been recorded the inspection method of ISDN nitrate, and what the method adopted is brown ring test detection method.Jiang Hua etc. have delivered the paper of " reversed-phase high-performance liquid chromatography is measured nitrate radical and the nitrite anions in water simultaneously " on " analytical chemistry " the 29th volume in July calendar year 2001, also disclose the method for utilizing chromatography determination nitrate radical.But meet the inflammable and explosive character of acid in view of monobel heat, can not adopt the nitrate detection method of above-mentioned routine to detect.Pharmacopeia both domestic and external, comprises American Pharmacopeia, British Pharmacopoeia, European Pharmacopoeia, Pharmacopeia of Japan and Chinese Pharmacopoeia, and other documents and materials, does not all record the detection method of medicinal nitroglycerin solution nitrate.Caused thus medicinal nitroglycerin solution nitrate detection method for many years in space state, be also that people in the industry wishes the technical barrier being resolved very much simultaneously.
Summary of the invention
The for many years research of inventor based on to this technical matters, thinks that if carry out the detection of nitroglycerin solution nitrate, key is to find a kind of scientific and reasonable pre-treating method.Nitroglycerin solution is inflammable and explosive substances, and easily degraded generates the accessory substances such as dinitric acid glyceride, a glycerin trinitrate and nitrate.Nitrate is soluble in water, and common solvent absolute ethyl alcohol and the water of nitroglycerin solution dissolve each other.According to the chemical property of above related substances, the pre-treating method that inventor provides a kind of nitroglycerin solution nitrate to detect, easily nitrate is separated from nitroglycerin solution, successfully avoid adopting conventional nitrate detection method to cause the inflammable and explosive fried situation of monobel.
The pre-treating method that described nitroglycerin solution nitrate detects comprises the steps:
(1) volatilize solvent: under room temperature normal pressure state of nature or room temperature decompression state, volatilize the solvent of described nitroglycerin solution sample to be checked, obtain residue for subsequent use;
(2) separated and dissolved nitrate: add purified water in described residue, jolting makes purified water fully contact with residue, places layering, gets after the filtration of upper water liquid, and filtrate is for subsequent use.
After above-mentioned pre-treatment, separate the filtrate obtaining and can be used for conventional nitrate detection, comprise existing nitrate brown ring test detection method and nitrate chromatographic detection.
Described nitroglycerin solution is ethanol solution or the monobel diethyl ether solution of monobel.
Further, the present invention also provides a kind of detection method of nitroglycerin solution nitrate, it is characterized in that comprising the following steps:
(1) volatilize solvent: take concentration and be 1 gram of 10% nitroglycerin solution, under room temperature atmospheric pressure state or room temperature decompression state, naturally volatilize the solvent of described detection sample, obtain residue for subsequent use;
(2) separated and dissolved nitrate: add 10 milliliters of purified water in described residue, jolting makes purified water fully contact with residue, places layering, and filtrate is for subsequent use afterwards to get the filtration of upper water liquid;
(3) nitrate brown ring test: get above-mentioned filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meeting place of boundary must not show brown immediately.
The present invention is with respect to its advantage of prior art:
1, the nitrate that present invention is directed at nitroglycerin solution detects, particularly the detection of the nitrate of medicinal nitroglycerin solution is a ground-breaking technology, this technology has been filled up the blank of medicinal nitroglycerin solution nitrate inspection technology, has successfully got rid of the situation that adopts conventional nitrate detection method to cause monobel burning or blast.
2, high, the good stability of detection method accuracy of the present invention.In pre-treatment step, volatilizing solvent is under the strong acid reagent effect of adding for fear of the monobel being dissolved in solvent, degradation reaction to occur in nitrate brown ring test inspection, the impact of the nitrate of generation on check result.Routine volatilizes solvent and adopts more the mode of heating, the present invention adopts room temperature naturally to volatilize the decompression of solvent or room temperature to volatilize the method for solvent, the one, in the situation that being heated, there is burning or blast for fear of monobel, also avoided on the other hand monobel to generate nitrate in the lower generation degraded of being heated, on the impact of check result.As can be seen here, detection method of the present invention is to design for the special nature of nitroglycerin solution, and not only specificity is simple to operate by force, and has got rid of in theory the disturbing factor of links, and good stability, accuracy are high.
3, because the brown ring test inspection of nitrate is the token test of nitrate, specificity and sensitivity are better, and have simple to operate, short advantage consuming time.After pre-treatment step of the present invention, then the brown ring test inspection of carrying out nitrate is particularly suitable for the production inspection operation of scale.
Embodiment
1. nitrate positive control test
The test of nitrate positive control adopts potassium nitrate.
Linear: to get dried potassium nitrate, add purified water and be made into containing NO
3 -concentration is 0.24mg/ml, 0.32 mg/ml, 0.4 mg/ml, 0.48 mg/ml, get 5ml and test by method, visual inspection, show brown substantially linear.
Minimum detectable level: nitrate (NO
3 -) minimum detection be limited to 0.24mg/ml.
2. the detection of nitroglycerin solution nitrate
091110 batch of nitroglycerin solution (10%) 1g of ①Qu Guangzhou Baiyunshan Mingxing Pharmaceutical Co., Ltd. (calling " Ming Xing company " in the following text) product, under room temperature, naturally volatilize after absolute ethyl alcohol (along with the volatilization of ethanol, solution becomes muddy by clarifying, after ethanol volatilizees totally completely, solution becomes again clarification), add purified water 10ml jolting 5 minutes, and place make layering, get upper water liquid filter, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meet place of boundary not aobvious brown.This batch products nitrate conforms with the regulations.
091111 batch of nitroglycerin solution of ②Qu Mingxing company product (10%) 1g, decompression under room temperature (pressure is-0.01MPa) volatilizes after absolute ethyl alcohol (along with the volatilization of ethanol, solution becomes muddy by clarifying, after ethanol volatilizees totally completely, solution becomes again clarification), add purified water 10ml jolting 5 minutes, and place make layering, get upper water liquid filter, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meet place of boundary not aobvious brown.This batch products nitrate conforms with the regulations.
091112 batch of nitroglycerin solution of ③Qu Mingxing company product (10%) 1g, decompression under room temperature (pressure is-0.06MPa) volatilizes after absolute ethyl alcohol (along with the volatilization of ethanol, solution becomes muddy by clarifying, after ethanol volatilizees totally completely, solution becomes again clarification), add purified water 10ml jolting 5 minutes, and place make layering, get upper water liquid filter, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meet place of boundary not aobvious brown.This batch products nitrate conforms with the regulations.
4. get Beijing Yi Min company 0910005 batch of nitroglycerin solution of product (10%) 1g, under room temperature, naturally volatilize after absolute ethyl alcohol that (along with the volatilization of ethanol, solution becomes muddy by clarifying, after ethanol volatilizees totally completely, solution becomes again clarification), add purified water 10ml jolting 5 minutes, and place make layering, get upper water liquid filter, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meet place of boundary not aobvious brown.This batch products nitrate conforms with the regulations.
5. get Beijing Yi Min company 0910006 batch of nitroglycerin solution of product (10%) 1g, decompression under room temperature (pressure is-0.01MPa) volatilizes after absolute ethyl alcohol (along with the volatilization of ethanol, solution becomes muddy by clarifying, after ethanol volatilizees totally completely, solution becomes again clarification), add purified water 10ml jolting 5 minutes, and place make layering, get upper water liquid filter, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, meet place of boundary not aobvious brown.This batch products nitrate conforms with the regulations.
091112 batch of nitroglycerin solution of ⑥Qu Mingxing company product (10%) 1g, under room temperature, natural volatile fraction absolute ethyl alcohol to solution becomes muddy by clarifying, and add purified water 10ml jolting 5 minutes, and placement makes layering, getting upper water liquid filters, get filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add ferrous sulphate test solution 5ml along tube wall, make into two liquid levels, connect the aobvious brown ring in place of boundary.Originally experimental results show that monobel is dissolved in absolute ethyl alcohol, in the time that absolute ethyl alcohol does not volatilize completely, be dissolved in monobel in absolute ethyl alcohol under the effect of strong acid sulfuric acid, produce degraded, generate nitrate, thereby disturbed test.
Claims (2)
1. the pre-treating method that the nitrate of nitroglycerin solution detects, is characterized in that comprising the following steps:
(1) volatilize solvent: under room temperature atmospheric pressure state or room temperature decompression state, naturally volatilize the solvent of described nitroglycerin solution sample to be checked, obtain residue for subsequent use;
(2) separated and dissolved nitrate: add purified water in described residue, jolting makes purified water fully contact with residue, places layering, gets upper water liquid and filters, and filters for conventional nitrate and detects test;
Wherein, described nitroglycerin solution is monobel ethanol solution, described in the terminal point determining method that volatilizes be: along with the volatilization of ethanol, solution becomes muddy by clarifying, when ethanol volatilize completely clean after, solution becomes again clarification.
2. a detection method for the nitrate of nitroglycerin solution, is characterized in that comprising the following steps:
(1) volatilize solvent: under room temperature atmospheric pressure state or room temperature decompression state, naturally volatilize the solvent of described nitroglycerin solution sample to be checked, obtain residue for subsequent use;
Wherein, described nitroglycerin solution is monobel ethanol solution, described in the terminal point determining method that volatilizes be: along with the volatilization of ethanol, solution becomes muddy by clarifying, when ethanol volatilize completely clean after, solution becomes again clarification;
(2) separated and dissolved nitrate: add purified water in described residue, jolting makes purified water fully contact with residue, places layering, gets upper water liquid and filters, and filters for conventional nitrate and detects test;
(3) nitrate brown ring test: get above-mentioned filtrate 5ml and be placed in test tube, add sulfuric acid 5ml, mix, let cool, slowly add copperas solution 5ml along closing, make into two liquid levels, meeting place of boundary must not show brown immediately.
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Citations (3)
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| EP1731548A1 (en) * | 2005-06-09 | 2006-12-13 | Commissariat A L'energie Atomique | Use of fluorescent polysiloxanes in chemical sensors for detection or dosage of nitrated compounds |
| ES2339368T3 (en) * | 2004-10-07 | 2010-05-19 | Commissariat A L'energie Atomique | CHEMICAL SENSORS UNDERSTANDING POLYLILOXANES WITH ANILINE AS SENSITIVE MATERIALS AND THEIR USE FOR DETECTION OR ASSESSMENT OF NITRATED COMPOUNDS. |
| CN102305833A (en) * | 2011-07-29 | 2012-01-04 | 中国烟草总公司郑州烟草研究院 | Measurement method of content of nitrites in polypropylene tow for cigarettes |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2339368T3 (en) * | 2004-10-07 | 2010-05-19 | Commissariat A L'energie Atomique | CHEMICAL SENSORS UNDERSTANDING POLYLILOXANES WITH ANILINE AS SENSITIVE MATERIALS AND THEIR USE FOR DETECTION OR ASSESSMENT OF NITRATED COMPOUNDS. |
| EP1731548A1 (en) * | 2005-06-09 | 2006-12-13 | Commissariat A L'energie Atomique | Use of fluorescent polysiloxanes in chemical sensors for detection or dosage of nitrated compounds |
| CN102305833A (en) * | 2011-07-29 | 2012-01-04 | 中国烟草总公司郑州烟草研究院 | Measurement method of content of nitrites in polypropylene tow for cigarettes |
Non-Patent Citations (5)
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| A. Daiber et.al..Mitochondrial aldehyde dehydrogenase (ALDH-2)—Maker of and marker for nitrate tolerance in response to nitroglycerin treatment.《Chemico-Biological Interactions》.2008,全文. * |
| 刘贤杰等.离子色谱法测定油基切削液和机床排泄物中的亚硝酸根.《广东化工》.2009,第36卷(第4期),2.1.1节第2段. * |
| 刘贤杰等.离子色谱法测定油基切削液和机床排泄物中的亚硝酸根.《广东化工》.2009,第36卷(第4期),参见2.1.1节第2段. * |
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