CN102759476A - Preparation method of cocaine hydrochloride standard substance - Google Patents
Preparation method of cocaine hydrochloride standard substance Download PDFInfo
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- CN102759476A CN102759476A CN2012102524587A CN201210252458A CN102759476A CN 102759476 A CN102759476 A CN 102759476A CN 2012102524587 A CN2012102524587 A CN 2012102524587A CN 201210252458 A CN201210252458 A CN 201210252458A CN 102759476 A CN102759476 A CN 102759476A
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Abstract
The invention belongs to a preparation method of a standard substance, and in particular relates to a preparation method of a cocaine hydrochloride standard substance. The invention solves the problems that in the prior art, the cocaine hydrochloride standard substance is high in impurity content, the preparation process of the standard substance is large in difference, the quality of the product is unstable, the preparation speed is low, the process is complex and the recovery rate is low, and provides a cocaine hydrochloride standard substance preparation method which is high in preparation speed and recovery rate and can obtain high-purity cocaine hydrochloride standard substances. The preparation method comprises the following steps of: preparing a cocaine hydrochloride sample solution and regulating the solution polarity; preparing and purifying the obtained sample solution by a medium-pressure preparation system; concentrating main-peak reception liquid obtained by preparing at reduced pressure to obtain a crude product of cocaine; preparing the crude product of cocaine into a solution, regulating the solution polarity, and purifying the obtained solution again; and concentrating the main-peak reception liquid obtained by preparing at reduced pressure to obtain the cocaine hydrochloride standard substance. The preparation method is simple in process and high in recovery rate, and is suitable for popularization and application.
Description
Technical field
The present invention relates to the reference material preparation method, more specifically, is a kind of preparation method of cocaine hydrochloride standard substance.
Background technology
Cocaine another name cocaine, human first kind of the natural alkaloid (C that finds with local anesthetic action
17H
21NO
4), be long-acting ester class local anaesthetics, fat-soluble height, penetration power is strong, and is good to the nerve fiber compatibility, can produce good surface anesthetic effect.Its pressor effect maybe be relevant to the reuptake of norepinephrine with the retardance nerve endings.Toxicity is bigger, and the excited cerebral cortex of ability produces floaty euphoria when low dose of, along with dosage increases, makes breathing, vasomotion and vomiting centre excited, and severe patient can be fainted from fear; The central respiration inhibition appears in heavy dose of inhibition that can cause the descending dissimilation of cerebral cortex, and suppresses cardiac muscle and cause heart failure.Cocaine absorbs from institute's application site (mucous membrane and intestines and stomach), and through the esterase hydrolyzed metabolism, metabolin is discharged through kidney at liver and blood plasma, and part also can be through the milk drainage.These article can pass through blood-brain barrier, and accumulate in central nervous system, and the drug concentration during acute poisoning in the brain is higher than blood concentration, and these article also can pass through placental barrier.Big and be easy to habituation because of its toxicity, replaced by other local anaesthetics recently.Its hydrochloride preparation commonly used clinically.
These article can be applicable to the local anaesthesia of various operations, are usually used in surgery anesthesias such as mouth, nose, pharynx, ear, urethra, vagina.
These article are mixed with 1%～10% WS, surface anesthesia, spraying, filling mucomembranous surface, dosage 30mg/ time.Surface anesthesia.The low dose of excited cerebral cortex of ability of using produces floaty euphoria, has very strong drug abuse potentiality and dependence.Heavy dose of application can make breathings, cardiovascular and vomiting centre is excited, and severe patient can be fainted from fear, and transfers inhibition to by excitement at last, respiration inhibition occurs, heart failure, even death.Can cause typical allergic reaction.Tissue is had certain pungency, can cause corneal clouding or ulcer, intraocular pressure can increase.Toxicity is big, should not inject in the body; The chance thermal decomposition was lost efficacy, unsuitable scalding; Should not share with adrenaline, the possibility that increases arrhythmia cordis and hypertensive crisis is arranged; Corneal has very strong detrimental effect, no longer uses as ophthalmology; Strong drug abuse potentiality are arranged, can produce dependence; These article are by administration of narcotic drug.
Standard items, promptly standard substance as a kind of criterion, is used for the medicine aspect, then is the standard content in the assay.
In the drug law enforcement investigation; Usually need use the cocaine standard substance the doubtful sample of cocaine of being captured is carried out qualitative, quantitative check evaluation; Have the cocaine standard substance now seldom, and because manufacturer is different, production technology is different; Cause the standard substance impurity content big and can't trace to the source, make a big impact for work such as the research of sample of cocaine, detections.
And slow, the complex process of the preparation speed of cocaine standard substance in the prior art, the recovery are low.
Summary of the invention
It is impure more to the objective of the invention is to overcome prior art cocaine hydrochloride standard substance; The preparation production technology difference of standard substance is big, unstable product quality, and preparation speed is slow; Agents useful for same is expensive; Complex process, the deficiency that the recovery is low provides a kind of preparation method who prepares that speed is fast, the recovery is high and can obtain high-purity cocaine hydrochloride standard substance.
Technical scheme of the present invention is summarized as follows:
A. prepare the cocaine hydrochloride sample solution, the adjustment solution polarity;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying;
C. the main peak for preparing is received the liquid concentrating under reduced pressure and obtain the cocaine bullion, this cocaine bullion is mixed with solution, the adjustment solution polarity, the solution that obtains passes through purifying once more;
D. the main peak for preparing is received the liquid concentrating under reduced pressure and obtain the cocaine hydrochloride standard substance.
Further, a kind of preparation method of cocaine standard substance may further comprise the steps:
A. being the sample of cocaine solution of 0.5-0.8g/ml with the methyl alcohol compound concentration, is that the ratio of 0.5-0.8g:1-2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.3-0.4g/ml; In the ratio of said sample and ethanol is that the ratio of 0.3-0.4g:1-2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity.
Preferred, a kind of preparation method of cocaine standard substance may further comprise the steps:
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:1-2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1-2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity.
The said amino of said amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups, and the specification of said filler is sphere or the indefinite form particle of 3-100 μ m.
Said moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, and twice condition of gradient elution is respectively: B increases to 100% by volumetric concentration 60% in 40min, keeps 100% wash-out 20min then; B increases to 20% by volumetric concentration 5% in 30min, keep 20% wash-out 10min then.
All need activating and regenerating after the each use of the chromatographic column that is adopted; Regeneration step is: with 5% formic acid-methanol solution with the 30ml/min flow velocity behind post 1h; With pure water with the 30ml/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with the 30ml/min flow velocity respectively towards post 30min.
Characteristics of the present invention are: 1, can remove the feasible preparation of unknown impuritie purifying good reproducibility in the cocaine hydrochloride sample; 2, has the advantage that preparation time is short, chromatographic column can reuse; 3, have that technology is simple, cost is low, the advantage of handling safety.The inventive method yield is high, and the good product quality product purity reaches more than 99%, properties of product good stability, suitable applying.
Description of drawings
Fig. 1 is the preparative chromatography figure of embodiment 1.
Embodiment
Below in conjunction with the practical implementation case the present invention is further described.
Embodiment 1:
With reference to Fig. 1, operate by following step:
A. take by weighing cocaine hydrochloride sample 6g, add the 15ml dissolve with methanol, make it to dissolve each other with the adjustment solution polarity to wherein adding the 15ml absolute ethyl alcohol again with moving phase.
B. the sample solution that step a is obtained injects compacting and is equipped with the systems produce purifying, and chromatographic condition is: 20-45 μ mHILIC chromatographic column, its filler are that secondary amine and tertiary amine mass ratio are the mixed fillers of 3:2; Mode with three series connection of 80g+80g+80g is provided with, and flow velocity 30ml/min detects wavelength 234nm; Auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution, and gradient condition is following:
Time (min) Start B% End B%
40 60 100
20 100 100
C. the 12-44min place is received liquid, promptly main peak receives liquid, collect the back in 40 ℃ of Rotary Evaporators ,-0.8 ~-0.95MPa concentrates down and obtains the cocaine bullion; Get this bullion 3.5g and add the 10ml dissolve with methanol, to wherein adding the 10ml absolute ethyl alcohol, this sample solution injection compacting is equipped with system carries out preparing the second time purifying again; Chromatographic condition is: 20-45 μ mHILIC chromatographic column, its filler are that secondary amine and tertiary amine mass ratio are the mixed fillers of 3:2, with three series system settings of 80g+80g+80g; Flow velocity 50ml/min; Detect wavelength 234nm, auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol; Gradient elution, gradient condition is following:
Time (min) Start B% End B%
30 5 ?20
10 20 20
D. the 13-17.4min place is received liquid, promptly main peak receives liquid, collect the back in 40 ℃ of Rotary Evaporators ,-0.8 ~-0.95Mpa concentrates down and obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, adopting gas chromatograph to detect its purity is 99.35%.
Chromatographic column is each all to need activating and regenerating after using, and regeneration step is: with 5% formic acid-methanol solution with 30m l/min flow velocity behind post 1h, with pure water with the 30ml/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with the 30ml/min flow velocity respectively towards post 30min.
Embodiment 2:
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:1.6ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators under 45 ℃, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1.6ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators under 45 ℃, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detecting its purity is 99.33%;
The said amino of said amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups; Filler is that primary amine, secondary amine and tertiary amine mass ratio are the mixed fillers of 1:1.5:1 in the present embodiment, and the specification of said filler is the sphere of 50-100 μ m.
Gradient condition is following:
Regeneration step is: with 5% formic acid-methanol solution with the 30ml/min flow velocity behind post 1h, with pure water with the 30ml/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with the 30ml/min flow velocity respectively towards post 30min.
Embodiment 3:
With the methyl alcohol compound concentration is the cocaine hydrochloride sample solution of 0.6g/ml, is that the ratio of 0.6g:1.2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators under 40 ℃, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1.4ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators under 40 ℃, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity, reaches 99.29%.
The said amino of said amino bonded silica filler is primary amine groups, and the specification of said filler is the indefinite form particle of 40-60 μ m.
Said moving phase: A is that chromatographically pure normal hexane, B are chromatographically pure ethanol, and twice condition of gradient elution is respectively: B increases to 100% by volumetric concentration 60% in 40min, keeps 100% wash-out 20min then; B increases to 20% by volumetric concentration 5% in 30min, keep 20% wash-out 10min then.
All need activating and regenerating after the each use of the chromatographic column that is adopted; Regeneration step is: with 5% formic acid-methanol solution with the 30ml/min flow velocity behind post 1h; With pure water with the 30ml/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with the 30ml/min flow velocity respectively towards post 30min.
Embodiment 4:
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:1ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators under 30 ℃, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators under 30 ℃, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity and reaches 99.32%.
The said amino of said amino bonded silica filler is secondary amine, and the specification of said filler is the sphere of 40-60 μ m.Condition of gradient elution is following:
Regeneration step is: with 5% formic acid-methanol solution with the 30ml/min flow velocity behind post 1h, with pure water with the 30ml/min flow velocity towards post 1h, use again methyl alcohol and absolute ethyl alcohol with the 30ml/min flow velocity respectively towards post 30min.
Embodiment 5:
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators under 55 ℃, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators under 55 ℃, concentrating under reduced pressure obtains the cocaine standard substance, nitrogen environment is preserved down, detects its purity and reaches 99.30%.
The said amino of said amino bonded silica filler is tertiary amine groups, and the specification of said filler is the sphere of 60-80 μ m.
Condition of gradient elution is the same.
The step of living again is the same.
Embodiment 6:
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:1-2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1-2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity and reaches 99.31%.
The said amino of said amino bonded silica filler is primary amine groups, and the specification of said filler is the indefinite form particle of 50-80 μ m.
Condition of gradient elution is the same.
The step of living again is the same.
The foregoing description only is some examples among the present invention, but not as to qualification of the present invention.
Claims (5)
1. the preparation method of a cocaine hydrochloride standard substance is characterized in that, may further comprise the steps:
A. prepare the cocaine hydrochloride sample solution, the adjustment solution polarity;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying;
C. the main peak for preparing is received the liquid concentrating under reduced pressure and obtain the cocaine bullion, this cocaine bullion is mixed with solution, the adjustment solution polarity, the solution that obtains passes through purifying once more;
D. the main peak for preparing is received the liquid concentrating under reduced pressure and obtain the cocaine hydrochloride standard substance.
2. the preparation method of a kind of cocaine hydrochloride standard substance according to claim 1 is characterized in that, may further comprise the steps:
A. being the cocaine hydrochloride sample solution of 0.5-0.8g/ml with the methyl alcohol compound concentration, is that the ratio of 0.5-0.8g:1-2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.3-0.4g/ml; In the ratio of said sample and ethanol is that the ratio of 0.3-0.4g:1-2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine standard substance, nitrogen environment is preserved down, detects its purity.
3. the preparation method of a kind of cocaine hydrochloride standard substance according to claim 2 is characterized in that,
A. being the cocaine hydrochloride sample solution of 0.6g/ml with the methyl alcohol compound concentration, is that the ratio of 0.6g:1-2ml adds ethanol adjustment solution polarity in the ratio of said sample and ethanol;
B. compacting in the sample solution process of step a acquisition is equipped with the systems produce purifying; Chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler, detects wavelength 234nm, auxiliary wavelength 280nm; Moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
C. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine bullion; This cocaine bullion is used the solution of methyl alcohol compound concentration as 0.35g/ml; In the ratio of said sample and ethanol is that the ratio of 0.35g:1-2ml adds ethanol adjustment solution polarity, the solution that obtains once more through in compacting be equipped with the systems produce purifying, chromatographic condition is: the filler of chromatographic column is the amino bonded silica filler; Detect wavelength 234nm; Auxiliary wavelength 280nm, moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol, gradient elution;
D. with the main peak for preparing receive liquid in Rotary Evaporators in 30-55 ℃ under, concentrating under reduced pressure obtains the cocaine hydrochloride standard substance, nitrogen environment is preserved down, detects its purity.
4. the preparation method of a kind of cocaine hydrochloride standard substance according to claim 2; It is characterized in that; The said amino of said amino bonded silica filler is primary amine groups, secondary amine or tertiary amine groups, and the specification of said filler is sphere or the indefinite form of 3-100 μ m.
5. the preparation method of a kind of cocaine hydrochloride standard substance according to claim 2; It is characterized in that; Said moving phase: A is that chromatographically pure normal hexane, B are the chromatographically pure absolute ethyl alcohol; Twice condition of gradient elution is respectively: B increases to 100% by volumetric concentration 60% in 40min, keeps 100% wash-out 20min then; B increases to 20% by volumetric concentration 5% in 30min, keep 20% wash-out 10min then.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107101864A (en) * | 2017-05-08 | 2017-08-29 | 公安部物证鉴定中心 | Method for preparing purified for the cocainehydrochloride standard substance of forensic science illicit drugs inspection |
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| CN1979127A (en) * | 2006-12-18 | 2007-06-13 | 中国矿业大学(北京) | Improved method for quick detection of Ramaria root spore density |
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| CN102565260A (en) * | 2011-12-20 | 2012-07-11 | 公安部禁毒情报技术中心 | Method for preparing diacetylmorphine hydrochloride standard substance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005095003A (en) * | 2003-09-03 | 2005-04-14 | Fuji Photo Film Co Ltd | Method for separating and purifying nucleic acid |
| CN1979127A (en) * | 2006-12-18 | 2007-06-13 | 中国矿业大学(北京) | Improved method for quick detection of Ramaria root spore density |
| CN102243155A (en) * | 2011-04-13 | 2011-11-16 | 西安理工大学 | Method for extracting residual veterinary drugs from environmental water sample or animal derived food |
| CN102565260A (en) * | 2011-12-20 | 2012-07-11 | 公安部禁毒情报技术中心 | Method for preparing diacetylmorphine hydrochloride standard substance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107101864A (en) * | 2017-05-08 | 2017-08-29 | 公安部物证鉴定中心 | Method for preparing purified for the cocainehydrochloride standard substance of forensic science illicit drugs inspection |
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Application publication date: 20121031 |