CN106093233A - The assay method of content of isomer in esomeprazole sodium freeze-dried powder injection - Google Patents
The assay method of content of isomer in esomeprazole sodium freeze-dried powder injection Download PDFInfo
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Abstract
The invention discloses and a kind of measure the high performance liquid chromatography of content of isomer in esomeprazole lyophilized injectable powder, wherein use polysaccharide derivates class chiral chromatographic column to detect；Flowing used is by C mutually3‑C8The ternary mixture system of linear paraffin, isopropanol, dehydrated alcohol composition；Flow velocity is 0.2 2.0ml/min；Detection wavelength is 302nm；Column temperature is 20 40 DEG C.The method has sample concentration advantage bigger, reproducible, lower-cost highly sensitive, applicable.
Description
Technical field
The present invention relates to a kind of method detecting esomeprazole content of isomer, be specifically related to a kind of for measuring Esso
The liquid chromatography of content of isomer in azoles sodium freeze-dried powder injection draws in U.S.A.
Background technology
Esomeprazole sodium is the sodium salt of the S-optical isomer of omeprazole, is the suppression of global first isomer proton pump
Agent (PPI), reduces gastric acid secretion by specificity suppression parietal cell proton pump.Demonstrate,prove through a large amount of clinical experiments and drug research
Real: the time of its maintenance gastric pH > 4 is longer, and acid suppression is in hgher efficiency, and curative effect is better than front two generation PPI, and individual variation is little.As newly
Generation PPI, has been widely used in the many acid related disorders of clinical treatment.
Esomeprazole sodium English name: Esomeprazolesodium.Molecular formula: C17H18N3NaO3S, molecular weight is
367.41, No. CAS: 161796-78-7, for white powder.Chemical formula is 5-methoxyl group-2-((S)-((4-methoxyl group-3,5-two
Methyl-2-pyridine radicals) methyl) sulfinyl-1 H-benzimidazole sodium.Esomeprazole sodium isomer is white powder, chemical formula
For 5-methoxyl group-2-((R)-((4-methoxyl group-3,5-dimethyl-2-pyridine radicals) methyl) sulfinyl-1 H-benzimidazole sodium.
The molecular structural formula of esomeprazole isomer is as follows:
Owing to isomer can be produced during synthesis Esomeprazole sodium, therefore to it is former to improve Esomeprazole sodium
Material and the quality of lyophilized injectable powder, reduce the risk of clinical application, needs a kind of spirit of exploitation on the basis of current detection method badly
The liquid chromatography of sensitivity higher detection esomeprazole isomer, with quick, easy, detect Esomeprazole sodium efficiently
The content of isomer in raw material and lyophilized injectable powder.
The high performance liquid chromatography of detection esomeprazole magnesium isomer is had at present, with α 1 in American Pharmacopeia (USP35)
Acid glycoprotein is the chromatographic column (100mm × 4.0mm) of fixing phase, and flowing is phosphate-buffered salt-acetonitrile (V:V=15:85) mutually, inspection
Survey wavelength is 302nm；Flow velocity 0.6ml/min, need testing solution concentration is 0.03mg/ml.Through test, this method separating degree is preferable,
But the applicable sample concentration of alpha1 Acid glycoprotein chromatographic column relatively low (no more than 0.1mg/ml) so that test sample concentration is relatively low, causes
The detection range of this method is restricted.Meanwhile, the sensitivity of the method for United States pharmacopoeia specifications itself is very limited, does not reaches higher
Control of product quality requirement.It addition, chromatographic column used uses alpha1 Acid glycoprotein for fixing phase, the protein filling life-span is shorter, becomes
This is higher.
Therefore need badly foundation a kind of highly sensitive, be suitable for that sample concentration is relatively big, good stability, lower-cost detection side
Method, provides foundation for esomeprazole sodium raw materials and lyophilized injectable powder Quality advance.
Summary of the invention
The invention provides a kind of liquid phase color measuring content of isomer in esomeprazole sodium raw materials and lyophilized injectable powder
Spectrometry.The method is on the premise of separating degree and theoretical cam curve all meet the requirement of " Chinese Pharmacopoeia " version in 2015, under having
State advantage: highly sensitive, applicable sample concentration is bigger, reproducible, cost is relatively low.
The present invention uses content of isomer in liquid chromatography for measuring esomeprazole sodium raw materials and lyophilized injectable powder
Method includes:
Polysaccharide derivates class chiral chromatographic column is used to detect；Wherein flowing used is by C mutually3-C8Linear paraffin, different
The ternary mixture system of propanol, dehydrated alcohol composition；Flow velocity is 0.2-2.0ml/min；Detection wavelength is 302nm；Column temperature is
20-40℃。
Wherein:
In the flowing mutually of described ternary mixture system, cumulative volume 100% based on flowing phase is counted, the volume hundred of isopropanol
Proportion by subtraction in the range of 50% to 85%, preferably 60% to 70%, most preferably 65%.If the percent by volume of isopropanol is more than
85%, then flowing is met is thick because the viscosity of isopropanol is big, and mobility is little, is unfavorable for carrying out liquid chromatograph separation.
If the percent by volume of isopropanol is less than 50%, then the theoretical cam curve of main peak esomeprazole does not reaches " Chinese Pharmacopoeia "
The requirement of regulation in (version in 2015).
C in flowing mutually3-C8Linear paraffin, isopropanol, the preferred 25-35:60-70:4-6 of volume ratio of dehydrated alcohol, optimum
Select 30:65:5.
C3-C8Linear paraffin is understood to mean that the normal alkane containing 3 to 8 carbon atoms, such as n-propane, normal butane, just
Pentane, normal hexane, normal heptane, normal octane.Described C3-C8Linear paraffin is selected from mentioned above any one, the most own
Alkane.
Described polysaccharide derivates class chiral chromatographic column is understood to mean that employing has cellulose derivative on Silica Surface
Class, amylose class silica gel as the chiral chromatographic column of chiral stationary phase；The example of described cellulose derivative class is, such as
Cellulose-three (3,5-xylyl carbamate), cellulose-three (4-methyl benzoic acid ester), cellulose-three (4-toluene
Aminocarbamic acid ester)；The example of described amylose class is, such as amylose-three (3,5-xylyl carbamate).
In the methods of the invention, chiral chromatographic column preferably employs amylose-three (3,5-xylyl amino first on Silica Surface
Acid esters) silica gel as the chiral chromatographic column of chiral stationary phase, the most commercially available DAICEL CHIRALCEL AD-H.
The preferred 0.5-1.5ml/min of described flow velocity, more preferably 0.6-1.2ml/min, most preferably 0.8ml/min.
The column temperature of described chiral chromatographic column is preferably 25-38 DEG C, most preferably 35 DEG C.
In the methods of the invention, the need testing solution detected can be every 1 milliliter of solution containing Esomeprazole sodium 1mg,
Applicable sample concentration 0.1mg/ml more than the CHIRAL-AGP chromatographic column employed in American Pharmacopeia (USP35)；Additionally, for
For measuring the content of esomeprazole isomer, the quantitative limit concentration (0.016ug/ml) of the inventive method is American Pharmacopeia
(USP35) 1/3 times of the quantitative limit concentration (0.05ug/ml) in detection method.It is indicated above the inventive method and U.S.'s medicine
The detection method of allusion quotation (USP35) is compared, and assay method of the present invention can detect lower quantitative limit concentration and be applicable to bigger
Sample concentration, lower content of isomer can be measured, susceptiveness is more preferable.
Accompanying drawing explanation
Fig. 1 is the liquid chromatogram of the system suitability solution in embodiment 1.
Fig. 2 is the liquid chromatogram of the solution of the detection sensitivity in embodiment 2.
Fig. 3 is the liquid chromatogram of the need testing solution in embodiment 3.
Fig. 4 is the enlarged drawing of Fig. 3.
Fig. 5 is the liquid chromatograph of the system suitability solution of detection method in American Pharmacopeia (USP35) in comparative example 1
Figure.
Fig. 6 is the liquid chromatogram of the need testing solution in comparative example 2.
Detailed description of the invention
Assay method of the present invention follows the steps below:
1) to weigh esomeprazole sodium freeze dry appropriate for precision, add appropriate anhydrous alcohol solution and quantitatively dilution make every 1
The milliliter solution containing Esomeprazole sodium 0.2-2.0mg, the most every 1 milliliter of solution containing Esomeprazole sodium 1.0mg, as confession
Test sample solution；
2) to weigh omeprazole reference substance appropriate for precision, add appropriate anhydrous alcohol solution and quantitatively dilution make every 1 milliliter
Containing the solution of omeprazole 0.0005-0.05mg, the most every 1 milliliter of solution containing omeprazole 0.01mg is as system suitability
Solution；
3) take system suitability solution 10-30 μ l (preferably 20 μ l) and be directly injected into chromatograph of liquid, record chromatogram；
4) in system suitability solution chromatogram the separating degree at esomeprazole peak and esomeprazole isomer peak and
In the case of theoretical cam curve all meets the requirements, take need testing solution 10-30 μ l (preferably 20 μ l) and be directly injected into chromatograph of liquid,
Record chromatogram；
Wherein chromatographic condition is:
Chromatographic column: polysaccharide derivates class chiral chromatographic column, it is preferred to use have amylose-three (3,5-on Silica Surface
Xylyl carbamate) silica gel as the chiral chromatographic column of chiral stationary phase, the most commercially available DAICEL
CHIRALCEL AD-H。
Flowing phase: normal hexane: isopropanol: the preferred 25-35:60-70:4-6 of volume ratio, most preferably 30:65 of dehydrated alcohol:
5；
Detection wavelength: 302nm；
Flow velocity: preferably 0.5-1.5ml/min, more preferably 0.6-1.2ml/min, most preferably 0.8ml/min；
Column temperature: be preferably 25-38 DEG C, most preferably 35 DEG C.
When calculating, the conversion of omeprazole reference substance is esomeprazole and the esomeprazole isomery of 50% of 50%
Body.The content of esomeprazole isomer is calculated according to area normalization method, different based on esomeprazole and esomeprazole
The peak area sum of structure body is 100% meter.Separating degree and theoretical cam curve are given by high performance liquid chromatograph.
Hereinafter with reference to accompanying drawing, the invention will be further described in conjunction with the embodiments, it is intended to is used for illustrating rather than limit
Determine the present invention.
Raw material and instrument
Esomeprazole sodium freeze-drying powder: Gansu Chengji Biopharmaceutical Co., Ltd..
Omeprazole reference substance: National Institute for Food and Drugs Control.
High performance liquid chromatograph: model Waters e2695.
Embodiment 1: system suitability
Chromatographic condition is as follows:
Chiral chromatographic column: DAICEL CHIRALCEL AD-H (250mm × 4.6mm, 5um)；
Flowing phase: normal hexane: isopropanol: dehydrated alcohol (volume ratio is 30:65:5)；
Detection wavelength: 302nm；
Flow velocity: 0.8ml/min；
Column temperature: 35 DEG C.
It is appropriate that precision weighs omeprazole reference substance, add appropriate anhydrous alcohol solution and quantitatively dilution make every 1 milliliter and contain
The solution of omeprazole 0.01mg, as system suitability solution.Take system suitability solution 20 μ l, be directly injected into liquid chromatograph
Instrument, record chromatogram (Fig. 1), result is shown in Table 1.
Table 1:
Above-mentioned separating degree and theoretical cam curve all meet " Chinese Pharmacopoeia " version in 2015 and require (separating degree >=1.5；Theoretical tower
Plate number >=2000).
Embodiment 2: sensitivity test
Use the chromatographic condition of embodiment 1.
It is appropriate that precision weighs omeprazole reference substance, add appropriate anhydrous alcohol solution and quantitatively dilution make every 1 milliliter and contain
The solution of omeprazole 0.5ug, as the solution of detection sensitivity.Take this solution 20 μ l, be directly injected into chromatograph of liquid, record
Chromatogram, as shown in Figure 2.
Result:
The signal to noise ratio (S/N) at esomeprazole peak and esomeprazole isomer peak is respectively 152 and 156.(see Fig. 2).
During calculating, the conversion of omeprazole reference substance is that esomeprazole and the esomeprazole isomer of 50% of 50%, i.e. Esso are beautiful
The concentration drawing azoles and esomeprazole isomer is 0.25ug/ml.
Detection limit (S/N=3) concentration of reckoning esomeprazole isomer and quantitative limit (S/N=10) concentration:
Detection limit concentration: 0.25ug/ml ÷ 156 × 3=0.005ug/ml
Quantitative limit concentration: 0.25ug/ml ÷ 156 × 10=0.016ug/ml
Embodiment 3: sample detection
Use the chromatographic condition of example 1.
Weigh esomeprazole sodium freeze dry 27.16mg, 27.25mg respectively, accurately weighed, put in 25ml measuring bottle respectively,
Add dehydrated alcohol make dissolving in right amount and be diluted to scale, shake up, make every 1 milliliter of solution containing Esomeprazole sodium 1mg, as
Need testing solution.
Esomeprazole peak and esomeprazole isomer peak separating degree and Esso in system suitability solution chromatogram
In the case of U.S.A draws the theoretical cam curve at azoles peak to meet the requirements, take need testing solution 20 μ l, be directly injected into chromatograph of liquid, record
Chromatogram, as shown in Figure 3 and Figure 4.
Result:
The content of esomeprazole isomer is calculated, based on esomeprazole and esomeprazole isomery by area normalization method
The peak area sum of body is 100% meter.Result shows, in two parts of need testing solutions, esomeprazole content of isomer is respectively
0.008% and 0.007%, in esomeprazole sodium freeze-drying powder, the meansigma methods of esomeprazole content of isomer is
0.0075%.
Comparative example 1:
The system suitability of esomeprazole isomer detection method in American Pharmacopeia (USP35).
Chromatographic condition:
Chromatographic column: CHIRAL-AGP (100mm × 4.0mm) (classify: L41) by chromatographic column；
Flowing phase: acetonitrile-phosphate buffer (V:V=75:425)
Detection wavelength: 302nm；
Flow velocity: 0.6ml/min
Sample size: 20ul
Phosphate buffer: measure 1mol/L sodium dihydrogen phosphate 70ml and 0.5mol/L disodium hydrogen phosphate 20ml, add water dilute
Release to 1000ml, shake up, measure 250ml, be diluted with water to 1000ml, shake up, to obtain final product.
Diluent: measure 0.25mol/L sodium phosphate 11ml and 0.5mol/L disodium hydrogen phosphate 22ml, be diluted with water to
1000ml, shakes up, and to obtain final product.
Take omeprazole reference substance 2mg, put in 10ml measuring bottle, add diluent and make dissolving and be diluted to scale, shake up, then essence
Close measure 1ml, put in 50ml measuring bottle, add diluent and make dissolving and be diluted to scale, shake up, i.e. make every 1 milliliter and draw containing Aomei
The solution of azoles 0.004mg.Taking 20 μ l and inject chromatograph of liquid, record chromatogram (Fig. 5), result is shown in Table 2.
Table 2:
Sensitivity: the signal to noise ratio (S/N) of esomeprazole peak and esomeprazole isomer is respectively 205 and 402.Calculate
Time, the conversion of omeprazole reference substance is esomeprazole and the esomeprazole isomer of 50%, the i.e. esomeprazole of 50%
It is 0.002mg/ml with the concentration of esomeprazole isomer.
The detection limit concentration of reckoning esomeprazole isomer and quantitative limit concentration:
Detection limit concentration: 0.002mg/ml ÷ 402 × 3=0.015ug/ml
Quantitative limit concentration: 0.002mg/ml ÷ 402 × 10=0.05ug/ml
As can be seen here, the quantitative limit concentration (0.05ug/ml) of the method is about the quantitative limit concentration of the inventive method
(0.016ug/ml) 3 times, show that the susceptiveness of the inventive method is higher.
Comparative example 2:
Esomeprazole isomer detection method detection freeze-dried powder in American Pharmacopeia (USP35).
Use the chromatographic condition of comparative example 1.
Weigh esomeprazole sodium freeze dry 40.04mg, 40.17mg respectively, accurately weighed, put in 25ml measuring bottle respectively,
Add methanol 5ml and make dissolving, then add diluent (comparative example 1) and be diluted to scale, shake up；Precision measures 1ml again, puts 50ml amount
In Ping, add diluent (comparative example 1) and be diluted to scale, shake up, make every 1 milliliter and contain the molten of Esomeprazole sodium 0.03mg
Liquid, as need testing solution.As shown in Figure 6, two parts of need testing solutions all do not detect esomeprazole isomer.
As can be seen here, for the chromatographic in American Pharmacopeia (USP35) detection method, esomeprazole isomer
Quantitative limit concentration is 0.05ug/ml, and it is equivalent to need testing solution concentration (0.03mg/ml) in comparative example 2
0.17%, i.e. under this test sample concentration, the Min. of the content of the esomeprazole isomer that can be detected by is
0.17% (this numerical value the most just wanting close to the esomeprazole isomer limit 0.2% of the middle regulation of American Pharmacopeia (USP35)
Ask).By comparison, for the chromatographic in the detection method of the present invention, the quantitative limit concentration of esomeprazole isomer
(0.016ug/ml) 0.0016% of need testing solution concentration (1.0mg/ml) in embodiment 3 is equivalent to, i.e. at this test sample
Under concentration, the Min. of the content of the esomeprazole isomer that can be detected by is 0.0016%；And can by embodiment 3
Seeing, having recorded the meansigma methods of esomeprazole content of isomer in esomeprazole sodium freeze dry is 0.0075%, shows this
Bright method may be used for measuring the sample that content of isomer is lower.
Embodiment 4: the response rate and replica test
Use the chromatographic condition of embodiment 1.
Weigh omeprazole reference substance 20.18mg, 20.24mg respectively, accurately weighed, put respectively in 20ml measuring bottle, add nothing
Water-ethanol makes dissolving in right amount and is diluted to scale, shakes up；Precision measures 1ml again, puts respectively in 100ml measuring bottle, adds dehydrated alcohol
It is diluted to scale, shakes up, as reference substance solution；
Take respectively esomeprazole sodium freeze dry 26.75mg, 27.04mg, 26.87mg, 26.92mg, 27.11mg,
27.20mg, puts in 25ml measuring bottle respectively；Accurate any one above-mentioned omeprazole reference substance solution 6 measuring 0.5ml again
Part, it is separately added in above-mentioned 25ml measuring bottle, adds dehydrated alcohol and make dissolving in right amount and be diluted to scale, shake up, molten as test sample
Liquid.
In the case of system suitability meets the requirements, take reference substance solution, need testing solution 20 μ l, be directly injected into
Chromatograph of liquid is analyzed.
Appointing and take above-mentioned a need testing solution repetition sample introduction 6 times, (esomeprazole isomer contains 6 measured results
Amount) RSD be 0.52%.Above-mentioned 6 parts of need testing solutions are detected, by calculating the recovery of esomeprazole isomer
Rate is respectively 99.2%, 98.9%, 99.8%, 99.9%, 98.7%, 99.5%, and RSD is 0.49%.All meet " middle traditional Chinese medicines
Allusion quotation " version required (RSD≤2%) 2015 years.(during calculating, the conversion of omeprazole reference substance is the esomeprazole and 50% of 50%
Esomeprazole isomer.)
It is indicated above that the high performance liquid chromatography of the present invention has the advantage that accuracy is high, reproducible.
It should be pointed out that, for this technical staff, under the premise without departing from the principles of the invention, it is also possible to the present invention
Carrying out some improvement and modification, these improve and modify and fall under the scope of the present invention too.
Claims (8)
1. measure a high performance liquid chromatography for content of isomer in esomeprazole sodium freeze-dried powder injection, wherein:
Polysaccharide derivates class chiral chromatographic column is used to detect；Flowing used is by C mutually3-C8Linear paraffin, isopropanol, anhydrous
The ternary mixture system of ethanol composition；Flow velocity is 0.2-2.0ml/min；Detection wavelength is 302nm；Column temperature is 20-40 DEG C.
Assay method the most according to claim 1, the percent by volume of isopropanol of wherein flowing in mutually is 50% to 85%
In the range of, preferably 60% to 70%, most preferably 65%, cumulative volume based on flowing phase is 100% meter.
Assay method the most according to claim 1, wherein flow C in mutually3-C8Linear paraffin, isopropanol, dehydrated alcohol
Volume ratio is 25-35:60-70:4-6, preferably 30:65:5.
Assay method the most according to any one of claim 1 to 3, wherein said C3-C8Linear paraffin is appointed selected from following
Meaning one: n-propane, normal butane, pentane, normal hexane, normal heptane, normal octane；Preferably normal hexane.
Assay method the most according to claim 1, wherein polysaccharide derivates class chiral chromatographic column is for using at Silica Surface
On have cellulose derivative class, amylose class silica gel as the chiral chromatographic column of chiral stationary phase；Described cellulose derives
Species is selected from cellulose-three (3,5-xylyl carbamate), cellulose-three (4-methyl benzoic acid ester), cellulose-three
Any one in (4-tolylcarbamate)；Described amylose class is amylose-three (3,5-xylyl amino
Formic acid esters).
Assay method the most according to claim 5, wherein polysaccharide derivates class chiral chromatographic column is for using at Silica Surface
On have the silica gel chiral chromatographic column as chiral stationary phase of amylose-three (3,5-xylyl carbamate).
Assay method the most according to claim 1, wherein flow velocity is 0.5-1.5ml/min, more preferably 0.6-1.2ml/
Min, most preferably 0.8ml/min.
Assay method the most according to claim 1, wherein the column temperature of chiral chromatographic column is 35 DEG C.
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| CN108181392A (en) * | 2017-12-23 | 2018-06-19 | 徐艳 | A kind of method of enantiomter in separation detection Omeprazole |
| CN112305125A (en) * | 2020-10-31 | 2021-02-02 | 湖南方盛制药股份有限公司 | Method for analyzing omeprazole by high performance liquid chromatography |
| CN112666304A (en) * | 2019-10-15 | 2021-04-16 | 扬子江药业集团有限公司 | Method for detecting enantiomer in esomeprazole sodium medicine |
| CN115791995A (en) * | 2022-09-09 | 2023-03-14 | 宜昌东阳光长江药业股份有限公司 | Detection method of esomeprazole sodium isomer for injection |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181392A (en) * | 2017-12-23 | 2018-06-19 | 徐艳 | A kind of method of enantiomter in separation detection Omeprazole |
| CN112666304A (en) * | 2019-10-15 | 2021-04-16 | 扬子江药业集团有限公司 | Method for detecting enantiomer in esomeprazole sodium medicine |
| CN112305125A (en) * | 2020-10-31 | 2021-02-02 | 湖南方盛制药股份有限公司 | Method for analyzing omeprazole by high performance liquid chromatography |
| CN115791995A (en) * | 2022-09-09 | 2023-03-14 | 宜昌东阳光长江药业股份有限公司 | Detection method of esomeprazole sodium isomer for injection |
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Application publication date: 20161109 |