CN107064376A - A kind of method of pseudomorphine content in detection opium tincture - Google Patents
A kind of method of pseudomorphine content in detection opium tincture Download PDFInfo
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- CN107064376A CN107064376A CN201611204081.2A CN201611204081A CN107064376A CN 107064376 A CN107064376 A CN 107064376A CN 201611204081 A CN201611204081 A CN 201611204081A CN 107064376 A CN107064376 A CN 107064376A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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Abstract
A kind of method for being applied to pseudomorphine content in detection opium tincture in analysis field, the detection method comprises the following steps：Chromatographic condition：Chromatographic column：Octadecylsilane chemically bonded silica is the C18 posts of filler, 5 μm of particle diameter；Column temperature：30 DEG C~40 DEG C；Flow velocity：1.3ml/min~1.7ml/min；Detection wavelength：230nm；Sample size：The μ l of 10 μ l~25；Mobile phase：Heptane sulfonic acid sodium salt and methanol；The invention is detected by this method detection there is reagent to be easy to get, instrument uses the low advantage of extensive, easy to operate, testing cost using HPLC methods.
Description
Technical field
The present invention relates to the method for pseudomorphine content in a kind of detection opium tincture in Pharmaceutical Analysis field.
Background technology
Opium tincture, English entitled Opium Tincture, the product is brown liquid, and volume foam can be played with water shaking.
It is even to be used to suffer from diarrhoea suitable for various acute intense pains, antibechic.Its main composition is morphine, and morphine is in illumination, oxidation, again
The larger pseudomorphine of toxicity can be produced under metal ion and alkalescence condition, therefore, pseudomorphine in a kind of opium tincture is developed
The detection method of content is always new problem urgently to be resolved hurrily.
The content of the invention
It is an object of the invention to provide a kind of detection method of pseudomorphine content in opium tincture, this method uses HPLC methods
(concentration, Gradient Elution Method) is detected, there is this method reagent to be easy to get, instrument is low using extensive, easy to operate, testing cost
The advantages of.
The object of the present invention is achieved like this：The method of pseudomorphine content, the detection method in a kind of detection opium tincture
Comprise the following steps：
(1) chromatographic condition：
Chromatographic column：Octadecylsilane chemically bonded silica post, specification 150 × 4.6mm, 5 μm
Column temperature：30 DEG C~40 DEG C
Flow velocity：1.3ml/min~1.7ml/min
UV-detector wavelength：230nm
Sample size：The μ l of 10 μ l~25
Mobile phase：Heptane sulfonic acid sodium salt and methanol
(2) preparation of sodium heptanesulfonate：
Sodium heptanesulfonate 1.1g is taken, the 1000ml that adds water dissolvings adjust pH to 2.6 ± 0.1 with 50% phosphoric acid solution；
(3) preparation of need testing solution：
Precision measures opium tincture 25ml, puts in 100ml measuring bottles, is diluted to scale with 1% acetum, shakes up, is used as confession
Test sample solution；
(4) preparation of contrast solution：
Precision measures need testing solution 1ml, puts in 100ml measuring bottles, plus 1% acetum is diluted to scale, shakes up；It is accurate
2ml is measured, is put in 10ml measuring bottles, scale is diluted to 1% acetum, shakes up as contrast solution；
(5) prepared by system suitability solution
Take morphine hydrochloride reference substance appropriate, be dissolved in water, the solution containing 0.2mg in every 1ml is made, 5ml is measured, plus
0.4% liquor ferri trichloridi 1ml, puts in boiling water bath and heats 10 minutes, let cool, be used as system suitability solution；
(6) assay method：
Precision measures the μ l of μ l of system suitability solution 10~25 injection liquid chromatographs, records chromatogram, the reservation of morphine
Time is 12-17 minute, and the relative retention time of pseudomorphine is that the separating degree between 1.7~2.0, each chromatographic peak should be greater than
1.5；Precision measures the μ l injection liquid chromatographs of contrast solution and the μ l of need testing solution 10~25 respectively, records chromatogram, calculates
The content of pseudomorphine；
(7) calculation formula
In formula：
AIt is right：Contrast solution main peak area；
APseudomorphine：Pseudomorphine peak area in need testing solution；
fPseudomorphine：Pseudomorphine correction factor, 0.25.
Mobile phase heptane sulfonic acid sodium salt and methanol use concentration, Gradient Elution Method in the assay method：The concentration,
Gradient Elution Method is following steps, and elution starts latter 0-2 minutes, heptane sulfonic acid sodium salt 85%, methanol 15%；After elution starts
2-38 minutes, heptane sulfonic acid sodium salt was by 85% to 50%, and methanol is by 15% to 50%；Elution starts latter 38-39 minutes, heptane
Sodium sulfonate solution is by 50% to 20%, and methanol is by 20% to 80%；Elution starts latter 39-53 minutes, heptane sulfonic acid sodium salt
20%, methanol 80%；Elution start it is latter 53-54 minutes, heptane sulfonic acid sodium salt by 20% to 85%, methanol by 80% to
15%；Elution starts latter 54-66 minutes, heptane sulfonic acid sodium salt 85%, methanol 15%.
The octadecylsilane chemically bonded silica post is selected from Agilent Eclipse XDB-C18 posts.
The present invention is characterized by its detection method, is detected using HPLC (concentration, Gradient Elution Method).
The detection method of pseudomorphine content compared with prior art, is easy to get, instrument is used with reagent in a kind of opium tincture
Extensively, the low advantage of easy to operate, testing cost, will be widely used in Pharmaceutical Analysis field.
Brief description of the drawings
Below in conjunction with the accompanying drawings and embodiment the present invention is described in detail.
Fig. 1 is the system suitability Solution H PLC collection of illustrative plates of the present invention.
Fig. 2 is the need testing solution HPLC collection of illustrative plates of the present invention.
Fig. 3 is the contrast solution HPLC collection of illustrative plates of the present invention.
Embodiment
Following instance will be helpful to the understanding to the present invention, but these examples to the present invention only for being illustrated, this hair
It is bright to be not limited to these contents.
Embodiment one
1. chromatographic condition
Chromatographic column：5 μm of 150 × 4.6mm of Agilent (Agilent) Eclipse XDB-C18, column temperature：30 DEG C~40 DEG C,
Flow velocity：1.3ml/min~1.7ml/min, Detection wavelength：230nm, sample size：The μ l of 10 μ l~25.
2. it is prepared by solution
2.1 mobile phase：Heptane sulfonic acid sodium salt and methanol
2.2 heptane sulfonic acid sodium salt：Sodium heptanesulfonate 1.1g is taken, the 1000ml that adds water dissolvings adjust pH with 50% phosphoric acid solution
To 2.6 ± 0.1.
2.3 need testing solution：Precision measures opium tincture 25ml, puts in 100ml measuring bottles, and quarter is diluted to 1% acetum
Degree, shakes up, is used as need testing solution.
2.4 contrast solution：Precision measures need testing solution 1ml, puts in 100ml measuring bottles, plus 1% acetum is diluted to quarter
Degree, shakes up；Precision measures 2ml, puts in 10ml measuring bottles, is diluted to scale with 1% acetum, shakes up as contrast solution.
2.5 system suitability solution：Morphine hydrochloride reference substance 20.69mg is weighed, is put in 100ml measuring bottles, with water dissolving simultaneously
Scale is diluted to, is shaken up；5ml is measured, the liquor ferri trichloridi 1ml for plus 0.4% puts in boiling water bath and heated 10 minutes, lets cool, and makees
For system suitability solution.
3. assay method
Using mobile phase heptane sulfonic acid sodium salt and methanol concentration, Gradient Elution Method；
Elution starts latter 0-2 minutes, heptane sulfonic acid sodium salt 85%, methanol 15%；Elution starts latter 2-38 minutes, heptane
Sodium sulfonate solution 85% → 50%, methanol 15% → 50%；Elution start it is latter 38-39 minutes, heptane sulfonic acid sodium salt 50% →
20%, methanol 20% → 80%；Elution starts latter 39-53 minutes, heptane sulfonic acid sodium salt 20%, methanol 80%；Elution starts
53-54 minutes afterwards, heptane sulfonic acid sodium salt 20% → 85%, methanol 80% → 15%；Elution starts latter 54-66 minutes, heptane
Sodium sulfonate solution 85%, methanol 15%.
3.1 system suitability
System suitability solution is taken, liquid chromatograph is injected；
The retention time of morphine is 15.058 minutes, and the relative retention time of pseudomorphine is point between 1.8, each chromatographic peak
2.0 are should be greater than from degree.
3.2 test samples are determined
Take need testing solution to inject liquid chromatograph, record collection of illustrative plates.
3.3 blank determination
Take contrast solution to inject liquid chromatograph, record collection of illustrative plates.
4. result of calculation
In formula：
AIt is right：Contrast solution main peak area；
APseudomorphine：Pseudomorphine peak area in need testing solution；
fPseudomorphine：Pseudomorphine correction factor, 0.25.
Test sample 1：
Test sample 2：
Test sample 3：
The selection of the flowing phase pH value of embodiment two
Other conditions be the same as Example one, mobile phase is used as using heptane sulfonic acid sodium salt and methanol nitrile.Sodium heptanesulfonate is molten
Liquid：Sodium heptanesulfonate 1.1g is taken, the 1000ml that adds water dissolvings adjust pH to 2.4 with 50% phosphoric acid solution.
The chromatographic peak of pseudomorphine is disturbed by other impurities peak in need testing solution, it is impossible to detected.
The selection of the mobile phase of embodiment three
Other conditions be the same as Example one, using mobile phase heptane sulfonic acid sodium salt and acetonitrile concentration, Gradient Elution Method；
Elution starts latter 0-2 minutes, heptane sulfonic acid sodium salt 85%, acetonitrile 15%；Elution starts latter 2-38 minutes, heptane
Sodium sulfonate solution 85% → 50%, acetonitrile 15% → 50%；Elution start it is latter 38-39 minutes, heptane sulfonic acid sodium salt 50% →
20%, acetonitrile 20% → 80%；Elution starts latter 39-53 minutes, heptane sulfonic acid sodium salt 20%, acetonitrile 80%；Elution starts
53-54 minutes afterwards, heptane sulfonic acid sodium salt 20% → 85%, acetonitrile 80% → 15%；Elution starts latter 54-66 minutes, heptane
Sodium sulfonate solution 85%, acetonitrile 15%.
The chromatographic peak of pseudomorphine is disturbed by other impurities peak in need testing solution, it is impossible to detected.
Claims (3)
1. a kind of method for detecting pseudomorphine content in opium tincture, it is characterised in that：The detection method comprises the following steps：
(1) chromatographic condition：
Chromatographic column：Octadecylsilane chemically bonded silica post, specification 150 × 4.6mm, 5 μm
Column temperature：30 DEG C~40 DEG C
Flow velocity：1.3ml/min~1.7ml/min
UV-detector wavelength：230nm
Sample size：The μ l of 10 μ l~25
Mobile phase：Heptane sulfonic acid sodium salt and methanol
(2) preparation of sodium heptanesulfonate：
Sodium heptanesulfonate 1.1g is taken, the 1000ml that adds water dissolvings adjust pH to 2.6 ± 0.1 with 50% phosphoric acid solution；
(3) preparation of need testing solution：
Precision measures opium tincture 25ml, puts in 100ml measuring bottles, is diluted to scale with 1% acetum, shakes up, is used as test sample
Solution；
(4) preparation of contrast solution：
Precision measures need testing solution 1ml, puts in 100ml measuring bottles, plus 1% acetum is diluted to scale, shakes up；Precision is measured
2ml, puts in 10ml measuring bottles, is diluted to scale with 1% acetum, shakes up as contrast solution；
(5) prepared by system suitability solution
Take morphine hydrochloride reference substance appropriate, be dissolved in water, the solution containing 0.2mg in every 1ml is made, measures 5ml, plus 0.4%
Liquor ferri trichloridi 1ml, puts in boiling water bath and heats 10 minutes, let cool, be used as system suitability solution；
(6) assay method：
Precision measures the μ l of μ l of system suitability solution 10~25 injection liquid chromatographs, records chromatogram, the retention time of morphine
For 12-17 minutes, the relative retention time of pseudomorphine was that the separating degree between 1.7~2.0, each chromatographic peak should be greater than 1.5；Point
Precision does not measure the μ l injection liquid chromatographs of contrast solution and the μ l of need testing solution 10~25, records chromatogram, calculates pseudomorphine
Content；
(7) calculation formula
In formula：
AIt is right：Contrast solution main peak area；
APseudomorphine：Pseudomorphine peak area in need testing solution；
fPseudomorphine：Pseudomorphine correction factor, 0.25.
2. a kind of method for detecting pseudomorphine content in opium tincture according to claim 1, it is characterised in that：It is described to determine
Mobile phase heptane sulfonic acid sodium salt and methanol use concentration, Gradient Elution Method in method：The concentration, Gradient Elution Method are as follows
Step, elution starts latter 0-2 minutes, heptane sulfonic acid sodium salt 85%, methanol 15%；Elution starts latter 2-38 minutes, heptane sulphur
Acid sodium solution is by 85% to 50%, and methanol is by 15% to 50%；Elution start it is latter 38-39 minutes, heptane sulfonic acid sodium salt by
50% to 20%, methanol is by 20% to 80%；Elution starts latter 39-53 minutes, heptane sulfonic acid sodium salt 20%, methanol 80%；
Elution starts latter 53-54 minutes, and heptane sulfonic acid sodium salt is by 20% to 85%, and methanol is by 80% to 15%；Elution starts rear 54-
66 minutes, heptane sulfonic acid sodium salt 85%, methanol 15%.
3. a kind of method for detecting pseudomorphine content in opium tincture according to claim 1, it is characterised in that：Described 18
Alkyl silane bonded silica gel column is selected from Agilent Eclipse XDB-C18 posts.
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Cited By (1)
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| CN108956798A (en) * | 2018-04-27 | 2018-12-07 | 青海省药品检验检测院 | A kind of morphine hydrochloride preparation content determining method |
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| CN108956798A (en) * | 2018-04-27 | 2018-12-07 | 青海省药品检验检测院 | A kind of morphine hydrochloride preparation content determining method |
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