CN102565260B - Method for preparing diacetylmorphine hydrochloride standard substance - Google Patents
Method for preparing diacetylmorphine hydrochloride standard substance Download PDFInfo
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- CN102565260B CN102565260B CN201110428554.8A CN201110428554A CN102565260B CN 102565260 B CN102565260 B CN 102565260B CN 201110428554 A CN201110428554 A CN 201110428554A CN 102565260 B CN102565260 B CN 102565260B
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Abstract
The invention discloses a method for preparing a diacetylmorphine hydrochloride standard substance. The method comprises the following steps of: preparing a methanol solution of a diacetylmorphine sample, and adding ethanol to adjust the polarity of the solution; performing preparation and purification by using a middle-pressure preparation system under the chromatographic conditions that a filler of a chromatographic column is an amino-bonded silica filler, a detection wavelength is 228 nm, an auxiliary wavelength is 215 nm, a mobile phase A is chromatographic pure normal hexane and a mobile phase B is chromatographic pure ethanol; performing gradient elution; concentrating reduced pressure concentration on main peak receiving liquid, which is prepared, in a rotary evaporator at the temperature of 30 to 55 DEG C to obtain the diacetylmorphine hydrochloride standard substance; and storing the diacetylmorphine hydrochloride standard substance in nitrogen environment, and detecting the purity of the diacetylmorphine hydrochloride standard substance. By adoption of the method, exposure of diacetylmorphine in air can be reduced, so hydrolytic spoilage of the diacetylmorphine is avoided, and the diacetylmorphine hydrochloride standard substance with high purity of over 99 percent is prepared. The method has the advantages of short preparation time, simple process, low cost and safety in operation, and the chromatographic column is reusable.
Description
Technical field
The present invention relates to a kind of preparation method of diacetylmorphine hydrochloride standard substance.
Background technology
Diacetylmorphine is a kind of narcotics, and its common form is diacetylmorphine hydrochloride.At present, China's forensic sciences at different levels laboratory mainly adopts chromatographic process to carry out to discover and seize the qualitative, quantitative inspection qualification work of diacetylmorphine sample.Therefore, want to obtain accurate, reliable expert's conclusion, must use diacetylmorphine hydrochloride standard substance.In addition, have traceability and the corresponding uncertainty of measurement of science in order to ensure analytical test result, forensic science laboratory, before carrying out analytical test, should adopt diacetylmorphine hydrochloride standard substance to confirm corresponding analysis test method.In addition, diacetylmorphine hydrochloride standard substance setting up the quality management system in laboratory, inspection research laboratory of court and staff's thereof ability, implement between laboratory the aspects such as value comparison, also play a very important role.
Present stage, domestic do not have research institution that diacetylmorphine hydrochloride standard substance can be provided, and the external diacetylmorphine hydrochloride standard substance of producing of import exists the problems such as costly, formality is loaded down with trivial details, the arrival cycle is long.At present, the qualitative, quantitative inspection qualification work of increasing diacetylmorphine sample is just being born in forensic sciences at different levels laboratory, for its analytical test level of General Promotion, strengthen accuracy and the confidence level of its inspection probation report of providing, just day by day urgent to the demand of diacetylmorphine hydrochloride standard substance.
That the present invention aims to provide is a kind of economical, diacetylmorphine hydrochloride standard substance preparation method fast and effectively, can make up the technological deficiency of China aspect diacetylmorphine hydrochloride standard substance development, improve domesticly relying on external situation completely in diacetylmorphine hydrochloride standard substance supply side; Simultaneously, the present invention will solve a difficult problem that lacks diacetylmorphine hydrochloride standard substance when diacetylmorphine sample qualitative, quantitative inspection qualification is carried out in forensic science laboratory, reduce research laboratory of court of basic unit the funds spending of buying diacetylmorphine hydrochloride standard substance.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide one to prepare the preparation method that speed is fast, can effectively avoid diacetylmorphine hydrolysis and acquisition high-purity (more than 99%) diacetylmorphine hydrochloride standard substance.
Technical scheme of the present invention is summarized as follows:
A preparation method for diacetylmorphine hydrochloride standard substance, comprises the following steps:
A. the diacetylmorphine sample solution taking methyl alcohol as solvent compound concentration as 0.5g/mL, the ratio that is 1g:1.5-2.3mL in described diacetylmorphine sample and the ratio of ethanol adds ethanol to adjust solution polarity;
B. in sample solution process step a being obtained, press preparation system to prepare purifying, chromatographic condition is: the filler of chromatographic column is amino bonded silica filler, detects wavelength 228nm, auxiliary wavelength 215nm, mobile phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, gradient elution; Gradient condition is as follows: B holder volume concentrations 15% wash-out 10min, in 40min, increase to 50% by volumetric concentration 15%, and then keep 50% wash-out 40min;
C. by the main peak receiving liquid preparing in Rotary Evaporators in 30-55 DEG C at, reduced pressure concentration obtains diacetylmorphine hydrochloride standard substance, under nitrogen environment, preserves, and detects its purity.
Described in described amino bonded silica filler, amino is primary amine groups, secondary amine or tertiary amine groups, and the specification of described filler is the spherical or indefinite form of 3-100 μ m.
Feature of the present invention is: 1, can reduce the aerial exposure of diacetylmorphine, thereby avoid diacetylmorphine hydrolytic spoilage, successfully prepare first more than 99% highly purified diacetylmorphine hydrochloride standard substance; 2, have advantages of that preparation time is short, chromatographic column can reuse; 3, there is the simple cost of technique low, the advantage of handling safety.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
A preparation method for diacetylmorphine hydrochloride standard substance, comprises the following steps:
A. accurately take diacetylmorphine sample 40mg, add methyl alcohol to 80 μ l and dissolve, then add wherein 80 μ l absolute ethyl alcohols to adjust solution polarity, make it to dissolve each other with mobile phase;
B. sample solution step a being obtained injects presses preparation system to prepare purifying, chromatographic condition is: 20-45 μ m HILIC chromatographic column (its filler is the mixed fillers that secondary amine and tertiary amine mass ratio are 3:2), tri-series connection of 12g+12g+12g, flow velocity 20ml/min, detect wavelength 228nm, auxiliary wavelength 215nm, mobile phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, gradient elution, gradient condition is as follows:
C. after 32-47min place receiving liquid (being main peak receiving liquid) being collected, under 50 DEG C of Rotary Evaporators ,-0.8～-0.95Mpa, concentrate and obtain diacetylmorphine hydrochloride standard substance, under nitrogen environment, preserve, adopting gas chromatograph to detect its purity is 99.58%.
Embodiment 2:
A preparation method for diacetylmorphine hydrochloride standard substance, comprises the following steps:
A. accurately take diacetylmorphine sample 100mg and add methyl alcohol to 200 μ l dissolving, then add wherein 150 μ l absolute ethyl alcohols to adjust solution polarity, make it to dissolve each other with mobile phase;
B. sample solution step a being obtained injects presses preparation system to prepare purifying, chromatographic condition is: 10 μ m HILIC chromatographic columns (its filler is the mixed fillers that the mass ratio of primary amine and secondary amine is 9:1), tri-series connection of 20g+20g+20g, flow velocity 30ml/min, detect the auxiliary wavelength 215nm of wavelength 228nm, mobile phase: A normal hexane (import chromatographically pure), B absolute ethyl alcohol (import chromatographically pure), gradient elution, gradient condition is as follows:
C. after 53.5-65min place receiving liquid (being main peak receiving liquid) being collected, under 50 DEG C of Rotary Evaporators ,-0.8～-0.95Mpa, concentrate and obtain hydrochloride standard substance, under nitrogen environment, preserve, adopt gas chromatograph to detect its purity 99.66%.
Embodiment 3:
A preparation method for diacetylmorphine hydrochloride standard substance, comprises the following steps:
A. accurately take sample 4g and add methyl alcohol and dissolve to 8ml, then add wherein 9.2ml absolute ethyl alcohol to make it to dissolve each other with mobile phase to adjust solution polarity;
B. sample solution step a being obtained injects presses preparation system to prepare purifying: 50-100 μ m HILIC chromatographic column (its filler is the mixed fillers that the mass ratio of secondary amine and tertiary amine is 3:2) tri-series connection of 80g+80g+80g, flow velocity 55ml/min, detect the auxiliary wavelength 215nm of wavelength 228nm, mobile phase: A normal hexane (import chromatographically pure), B absolute ethyl alcohol (import chromatographically pure), gradient elution, gradient condition is as follows:
C. after 60-75min place receiving liquid (being main peak receiving liquid) being collected, under 50 DEG C of Rotary Evaporators ,-0.8～-0.95Mpa, concentrate and obtain hydrochloride standard substance, under nitrogen environment, preserve, adopt gas chromatograph to detect its purity 99.64%.
Chromatographic column can activating and regenerating, and regeneration step is: rush after post 1h with 30mL/min flow velocity with the methanol solution containing 5% formic acid, rush post 1h with pure water with 30mL/min flow velocity, respectively rush post 30min with 30mL/min with methyl alcohol and absolute ethyl alcohol.
Claims (2)
1. a preparation method for diacetylmorphine hydrochloride standard substance, is characterized in that comprising the following steps:
A. the diacetylmorphine sample solution taking methyl alcohol as solvent compound concentration as 0.5g/mL, the ratio that is 1g:1.5-2.3mL in described diacetylmorphine sample and the ratio of ethanol adds ethanol to adjust solution polarity;
B. in sample solution process step a being obtained, press preparation system to prepare purifying, chromatographic condition is: the filler of chromatographic column is amino bonded silica filler, detects wavelength 228nm, auxiliary wavelength 215nm, mobile phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, gradient elution; Gradient condition is as follows: B holder volume concentrations 15% wash-out 10min, in 40min, increase to 50% by volumetric concentration 15%, and then keep 50% wash-out 40min;
C. by the main peak receiving liquid preparing in Rotary Evaporators in 30-55 DEG C at, reduced pressure concentration obtains diacetylmorphine hydrochloride standard substance, under nitrogen environment, preserves, and detects its purity.
2. the preparation method of a kind of diacetylmorphine hydrochloride standard substance according to claim 1, it is characterized in that amino described in described amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups, and the specification of described filler is the spherical or indefinite form of 3-100 μ m.
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| CN102759476A (en) * | 2012-07-20 | 2012-10-31 | 公安部禁毒情报技术中心 | Preparation method of cocaine hydrochloride standard substance |
| CN102749402A (en) * | 2012-08-07 | 2012-10-24 | 公安部禁毒情报技术中心 | Preparation method of morphine hydrochloride standard substance |
| CN107304213B (en) * | 2016-04-20 | 2021-08-20 | 李显林 | Method and equipment for processing poppy extract |
| CN107478733B (en) * | 2017-05-08 | 2019-03-12 | 公安部物证鉴定中心 | The method for preparing purified of codeine standard substance for forensic science illicit drugs inspection |
| CN107345946B (en) * | 2017-05-08 | 2019-11-01 | 公安部物证鉴定中心 | The method for preparing purified of methcathinone standard substance for forensic science illicit drugs inspection |
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| WO1999022244A2 (en) * | 1997-10-27 | 1999-05-06 | Varian, Inc. | Method for determination of drugs of abuse in biological samples |
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| CN101750458A (en) * | 2009-11-05 | 2010-06-23 | 香港科技大学 | Method for detecting drug residues in human body |
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| WO1999022244A2 (en) * | 1997-10-27 | 1999-05-06 | Varian, Inc. | Method for determination of drugs of abuse in biological samples |
| CN1818635A (en) * | 2006-03-15 | 2006-08-16 | 首都师范大学 | THz inspection and fingerprint spectrum for 12 drugs |
| CN101750458A (en) * | 2009-11-05 | 2010-06-23 | 香港科技大学 | Method for detecting drug residues in human body |
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