CN110031584A - The method that HPLC method measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese - Google Patents
The method that HPLC method measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese Download PDFInfo
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- CN110031584A CN110031584A CN201910307268.2A CN201910307268A CN110031584A CN 110031584 A CN110031584 A CN 110031584A CN 201910307268 A CN201910307268 A CN 201910307268A CN 110031584 A CN110031584 A CN 110031584A
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- benzalkonium chloride
- chinese
- nasal spray
- salmon calcitonin
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention belongs to analytical chemistry fields, and in particular to a kind of method that HPLC method measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese.The chromatographic column that the method uses is to carry out isocratic elution using the mobile phase A and Mobile phase B of optimization using octadecylsilane chemically bonded silica as filler；The drug is polypeptide nasal spray, and bacteriostatic agent is benzalkonium chloride.Method of the invention conveniently can accurately measure the content of bacteriostatic agent in polypeptide drug salmon calcitonin nasal spray in Chinese；Method of the invention is easy to operate, quick, accurate, high sensitivity, reproducible, mild condition, tailing factor are small, pass through the methodology validation of system, prove the measurement of this method benzalkonium chloride content suitable for salmon calcitonin nasal spray in Chinese, inspection result is accurate and reliable, for realizing that the quality control of salmon calcitonin nasal spray in Chinese has great importance.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to a kind of HPLC method analysis measurement salmon calcitonin nasal spray in Chinese benzene bundle
The method of oronain content.
Background technique
Salmon calcitonin nasal spray in Chinese is for treating osteoporosis, Paget ' s disease (scleromalacia), hypercalcinemia, height
The diseases such as blood calcium crisis and various ostalgia, achieve preferable effect during the last ten years, because its is significant in efficacy, Small side effects are cured
It works the favorable comment of author and patient.
Salmon calcitonin nasal spray in Chinese is aqueous solution type preparation, and benzalkonium chloride is its bacteriostatic agent, is able to suppress bacterial growth, from
And extend the shelf life of drug, while ensureing the safety of patient during use.Benzalkonium chloride contained in this product prescription is
Common bacteriostatic agent, dosage cross conference and generate certain inhibiting effect to the fibre swing of schneiderian membrane, and dosage deficiency is then not achieved
Therefore corresponding inhibitory effect for the quality for further controlling this product, establishes accurate easily bacteriostatic agent benzalkonium chloride containing measurement
The method of determining is extremely important.
Benzalkonium chloride easily trails as quaternary ammonium compound, chromatography appearance, and peak shape is poor, causes one to accurate quantitative analysis
Fixed difficulty.Prevent involved in existing version Chinese Pharmacopoeia neomycin sulfate ophthalmin solution in 2015 and Gernebcin eye drops quality standard
The detection of rotten agent benzalkonium chloride, but tailing factor is larger (about 1.5).
Summary of the invention
In view of this, the present invention provides benzalkonium chloride content in a kind of HPLC method analysis measurement salmon calcitonin nasal spray in Chinese
Method, can benzalkonium chloride content in Accurate Determining salmon calcitonin nasal spray in Chinese, and the method is easy to operate, quick, accurate, sensitive
Spend that high, reproducible, mild condition, tailing factor are small, and inspection result is accurate and reliable, for realization salmon calcitonin nasal spray in Chinese
Quality control has great importance.
To achieve the above object, technical scheme is as follows:
The method that HPLC method measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese, chromatographic column use octadecylsilane
Bonded silica gel is filler, YMC, model: TA12S05-2546WT.
The research of the invention finds that the chromatographic column using above-mentioned model can preferably realize benzene in salmon calcitonin nasal spray in Chinese
The separation of oronain and other compositions is pricked, peak shape is good, and tailing factor is small.The chromatographic column of the model uses organosilan and inorganic silicon
Alkane multilayer hybrid matrix particle, the closed-end technology that this silica gel particle uses can make the position for being easy reaction and be difficult to corrode non-
Activator combines, and can farthest block the silanol group for being difficult to react, to realize brilliance and resistance to
Long property and obtain good chromatographic peak profile.
Further, the mobile phase A that the above method uses adds 1.5% three second for 9~11mmol/L ammonium acetate aqueous solution
Amine, with glacial acetic acid tune pH to 5.0 ± 0.5；Mobile phase B is acetonitrile, isocratic with A:B=28~32:72~68 (volume ratio, v/v)
Elution.
Most preferably, mobile phase A is 10mmol/L ammonium acetate aqueous solution, adds 1.5% triethylamine, extremely with glacial acetic acid tune pH
5.0±0.5；Mobile phase B is acetonitrile；A:B=30:70 (volume ratio, v/v), isocratic elution.
The research of the invention finds that using existing method mobile phase, for example (mobile phase A (adds for 5mmol/L ammonium acetate aqueous solution
1% triethylamine (TEA), with glacial acetic acid tune pH to 5.0 ± 0.5), Mobile phase B is acetonitrile；A:B=35:65, isocratic elution) color
It composes peak easily to trail, peak shape is poor, causes accurate quantitative analysis certain difficulty.Further the study found that using the present invention
Mobile phase can improve the peak shape of benzalkonium chloride, reduce smearing, thus effectively by benzalkonium chloride and principal component and related
Impurity is separated, and achievees the purpose that more accurate quantitative analysis.Principle analysis is as follows: remaining slant acidity silanol on C18 Bonded Phase
Base is easy that peak is caused to take off tail with alkali compounds in conjunction with, so, being added after alkaline triethylamine in mobile phase can be first
In conjunction with silanol group, to hinder the effect of sample medium alkaline compound and silanol group, reduce peak hangover.Ammonium acetate belongs to
Ion-pairing agent, for the concentration of ion pair generally between 10-50mmol/L, different concentration has not the retention behavior of chromatography
The same influence, by screening ion concentration, the effect of winding up of available optimization.
Further, above-mentioned HPLC uses following condition:
Flow velocity: 0.8-1.2mL/min, preferably 1.0mL/min；
Detection wavelength: 262nm；
Column temperature: 35-45 DEG C, preferably 40 DEG C；
Sample volume: 20 μ l
It is that test sample is detected that above-mentioned HPLC method, which can directly adopt salmon calcitonin nasal spray in Chinese,.
Above-mentioned HPLC method further includes the preparation of benzalkonium chloride reference substance solution, benzalkonium chloride reference substance in the reference substance solution
Concentration is preferably 0.8% (v/v).Such as specific preparation method includes: accurate measurement benzalkonium chloride reference substance 0.4ml, sets 50ml
It in measuring bottle, is diluted with water to scale, shakes up to obtain the final product.
The method of the present invention is more targeted for the detection of quaternary ammonium salt preservative benzalkonium chloride, and detection effect is more preferably.
The method of the present invention is detected using UV detector.
Specifically, the method for benzalkonium chloride content includes: to take salmon in above-mentioned HPLC method measurement salmon calcitonin nasal spray in Chinese
Each 20 μ L of calcitonin nasal spray, benzalkonium chloride reference substance solution injects liquid chromatograph, is detected, is pressed by above-mentioned chromatographic condition
External standard method calculates benzalkonium chloride content.
Compared with prior art, the invention has the following beneficial effects:
(1) the method for the present invention test sample can directly adopt finished dosage form, and it is right in sample handling processes to can be effectively avoided
The consumption of bacteriostatic agent benzalkonium chloride, and unstable polypeptide drug degradation in sample handling processes is avoided to generate the dry of impurity
It disturbs.
(2) isocratic elution being carried out using the mobile phase that the present invention optimizes, analysis method good tolerance, baseline noise is small,
Sensitivity of analytical method is high；
(3) the method for the present invention can preferably realize that benzene is pricked in salmon calcitonin nasal spray in Chinese using the chromatographic column of specific model
The separation of oronain and other compositions, peak shape is good, and tailing factor is small；
(4) analysis method of the present invention column temperature compared with method reported in the literature is lower, and can increase chromatographic column uses the longevity
Life, chromatographic condition is milder, and it is convenient to operate；
(5) monitoring of bacteriostatic agent in salmon calcitonin nasal spray in Chinese is carried out using analysis method of the present invention, it is average to return
Yield is 100.1%, and relative standard deviation (RSD) is 1.15.The requirement such as system suitability: each peak separating degree meets regulation, benzene
Prick oronain tailing factor < 1.3.
Detailed description of the invention
Fig. 1 is 1 system suitability Solution H PLC of embodiment figure.
Fig. 2 is 1 benzalkonium chloride reference substance solution HPLC of embodiment figure.
Fig. 3 is 1 salmon calcitonin nasal spray in Chinese HPLC of embodiment figure.
Fig. 4 is 1 system suitability Solution H PLC of comparative example figure.
Fig. 5 is 1 benzalkonium chloride reference substance solution HPLC of comparative example figure.
Fig. 6 is 1 salmon calcitonin nasal spray in Chinese HPLC of comparative example figure.
Fig. 7 is 2 benzalkonium chloride reference substance solution HPLC of comparative example figure.
Fig. 8 is 2 salmon calcitonin nasal spray in Chinese HPLC of comparative example figure.
Specific embodiment
It detailed description of a preferred embodiment of the present invention will be given below.The reality of actual conditions is not specified in preferred embodiment
Proved recipe method, usually according to normal condition, illustrated embodiment are but not to be to preferably be illustrated to the contents of the present invention
The contents of the present invention are only limitted to illustrated embodiment.So those skilled in the art are according to foregoing invention content to embodiment party
Case carries out nonessential modifications and adaptations, still falls within protection scope of the present invention.
Instrument: 1260 type high performance liquid chromatograph (Anjelen Sci. & Tech. Inc) of Agilent；AB265-S type electronics point
It analyses balance (Mettler Toledo Inc.)；UV-1601 ultraviolet-uisible spectrophotometer (the limited public affairs of Beijing Rayleigh analysis instrument
Department).
Reagent:
Benzalkonium chloride reference substance (1.11%, w/v): National Institute for Food and Drugs Control, lot number: 100549-201102,
Containing benzalkonium chloride in every 1ml is 11.10mg, wherein containing n-C12H25Substitution homologue is 66.27%, n-C14H29Replace homologue
It is 33.33%.
Benzalkonium chloride (production is used): Shanghai Jinshan longitude and latitude Chemical Co., Ltd., lot number: 121002.
Salmon calcitonin nasal spray in Chinese: Yingu Pharmaceutical Co., Ltd., lot number: 1301012,1301022,1301032；
Salmon calcitonin raw material: Shanghai Soho-yiming Pharmaceuticals Co., Ltd., lot number: 1209011.
Ammonium acetate, triethylamine, glacial acetic acid are to analyze pure (Sinopharm Chemical Reagent Co., Ltd.)；Acetonitrile is chromatographically pure
(German Merck company).
The preparation of sample solution:
Test solution: finished dosage form is directly taken.
Benzalkonium chloride reference substance solution: precision measures benzalkonium chloride reference substance 0.4ml, sets in 50ml measuring bottle, is diluted with water
To scale, shake up to obtain the final product.
Benzalkonium chloride (preparation production is used) sample solution: it is pricked by the benzalkonium chloride in water that recipe quantity concentration is prepared as benzene
Oronain sample solution.
Salmon calcitonin solution: precision weighs salmon calcitonin about 10mg, sets in 10ml measuring bottle, is diluted with water to scale,
It shakes up to obtain the final product.
System suitability solution: measuring benzalkonium chloride contrast solution and salmon calcitonin solution 1:1 is mixed to obtain the final product.
Blank solution (contains main ingredient, be free of benzalkonium chloride): being prepared into the negative sample without benzalkonium chloride by recipe quantity, makees
For blank solution.
The method that 1 HPLC of embodiment measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese
Chromatographic condition:
Chromatographic column: C18 (4.6 × 250mm, 5 μm, 12nm), YMC, model: TA12S05-2546WT
Mobile phase: mobile phase A is 10mmol/L ammonium acetate aqueous solution, adds 1.5% triethylamine, extremely with glacial acetic acid tune pH
5.0±0.5；Mobile phase B is acetonitrile；A:B=30:70 (volume ratio, v/v), isocratic elution.
Flow velocity: 1.0mL/min；
Detection wavelength: 262nm；
Column temperature: 40 DEG C；
Sample volume: 20 μ l.
20 μ l of system suitability solution is taken to inject liquid chromatograph, the peak benzalkonium chloride C12 and the separating degree at the peak C14 should meet
It is required that the separating degree at the peak benzalkonium chloride C12 and salmon calcitonin peak should be greater than 1.5, and based on the peak benzalkonium chloride C12, tailing factor
It should be less than 1.5.
Benzalkonium chloride is the mixture of chlorodimethyl benzyl hydrocarbon ammonium, also referred to as dimethyl benzyl alkyl ammomium chloride
(shown in general structure following formula I, R is alkyl=C8H17~C18H37)), mainly by 3 kinds of homologue (dodecyl dimethyl benzyls
Ammonium chloride C12, myristyl benzyl dimethyl ammonium chloride C14With cetalkonium chloride C16) composition.We are logical
It crosses and benzalkonium chloride used in salmon calcitonin nasal spray in Chinese is detected, it is found that its homologous components is C12(R be alkyl=
C12H25), therefore we measure benzalkonium chloride content with C12Benzalkonium chloride (C21H38ClN) containing for index expression benzalkonium chloride
Amount.
Each 20 μ L injection liquid chromatograph of benzalkonium chloride reference substance solution, test sample salmon calcitonin nasal spray in Chinese is taken, by upper
It states chromatographic condition to be detected, by external standard method with calculated by peak area test sample benzalkonium chloride content.
By same procedure, the content of multiple batches of salmon calcitonin nasal spray in Chinese is detected.Testing result is as shown in the table:
| Batch | Benzalkonium chloride content |
| 1301012 | 93% |
| 1301022 | 94% |
| 1301032 | 93% |
System suitability solution chromatogram is shown in that Fig. 1, benzalkonium chloride reference substance solution HPLC figure are shown in Fig. 2, the spray of salmon calcitonin
Nose agent HPLC chromatogram is shown in Fig. 3 (lot number 1301022).
Comparative example 1
Compared with Example 1, difference, which is only that, replaces with common C18 column (the limited public affairs of Beijing enlightening section equine skill for chromatographic column
Department).Take each 20 μ L injection liquid phase of system suitability solution, benzalkonium chloride reference substance solution, test sample salmon calcitonin nasal spray in Chinese
Chromatograph is detected.Testing result is shown in Fig. 4 (system suitability Solution H PLC figure), Fig. 5 (benzalkonium chloride reference substance solution
HPLC figure), Fig. 6 (salmon calcitonin nasal spray in Chinese HPLC figure, lot number 1301022).The result shows that benzene is pricked using the C18 column of enlightening horse
Oronain peak shape is bad, and hangover is serious, and tailing factor is all larger than 1.5, shows that the control methods accurate quantitative analysis is poor.
Comparative example 2
Compared with Example 1, difference, which is only that, does following adjustment for chromatographic condition, and chromatographic column remains unchanged, and is still YMC
(model TA12S05-2546WT).
Chromatographic column: using octadecylsilane chemically bonded silica for filler, YMC, model: TA12S05-2546WT.Flow velocity:
1.0mL/min；Detection wavelength: 262nm；Column temperature: 30 DEG C；Sample volume: 20 μ l
Mobile phase: mobile phase A is 5mmol/L ammonium acetate aqueous solution, adds 1.5% triethylamine, with glacial acetic acid tune pH to 5.0
±0.5；Mobile phase B is acetonitrile；A:B=40:60, isocratic elution.
Each 20 μ L injection liquid chromatograph of benzalkonium chloride reference substance solution, test sample salmon calcitonin nasal spray in Chinese solution is taken,
It is detected by above-mentioned chromatographic condition, calculates the tailing factor at benzalkonium chloride peak in reference substance and test sample.Testing result is shown in Fig. 7
(benzalkonium chloride reference substance solution HPLC figure), Fig. 8 (salmon calcitonin nasal spray in Chinese HPLC figure, lot number 1301022), the results showed that though
Right YMC column performance is outstanding, but if chromatographic condition is not up to optimal conditions, benzalkonium chloride chromatographic peak still has biggish drag
The tail factor shows the method that the control methods is inferior in embodiment 1.
Experimental example methodology validation
If it is no it is special indicate, following chromatographic condition is the same as embodiment 1.
1, the measurement of maximum absorption wavelength
Benzalkonium chloride reference substance solution and salmon calcitonin solution is taken to be swept in 200-280nm wave-length coverage respectively
It retouches, determines that the wavelength at maximum absorption band is 262nm.
2, accuracy
It is accurate respectively to measure benzalkonium chloride reference substance solution, the rate of recovery 50%, the rate of recovery 100%, 150% sample of the rate of recovery
20 μ l inject liquid chromatograph, record chromatogram.
The rate of recovery is calculated (with n-C by following formula12H25Homologue is replaced to calculate).
A sample: the peak area of rate of recovery sample；A pairs: benzalkonium chloride compares peak area；C pairs: benzalkonium chloride reference substance solution
Concentration (mg/ml)；V: the constant volume (ml) of rate of recovery sample；V pairs: the measurement volume of rate of recovery sample benzalkonium chloride control
(ml)；X: the content of benzalkonium chloride control.
Acceptable standard are as follows: the average recovery rate under each concentration should all be between 98.0%-102.0%, 9 rate of recovery
The relative standard deviation (RSD) of data should be not more than 2.0%.
As a result it see the table below:
3, precision
Precision measures above-mentioned solution 5ml, sets in 10ml volumetric flask, is diluted with water to scale, shakes up, parallel to prepare 6 parts, point
The inaccurate 20 μ l that measure inject liquid chromatograph, record chromatogram.The benzalkonium chloride peak area of 6 parts of solution is (with n-C12H25Replace
Homologue meter) relative standard deviation less than 2.0%.
4, linearity and range
It is accurate respectively to measure above-mentioned 20 μ l of solution injection liquid chromatograph, record chromatogram.It is cross with benzalkonium chloride content
Coordinate, peak area are ordinate, carry out linear regression, obtain regression equation and related coefficient.Acceptable standard are as follows: the tropic
Related coefficient (R) cannot be less than 0.9990.
As a result it see the table below:
The concentration ranges that method is covered are at least the 80%~120% of labelled amount, according to accuracy and linear verification knot
Fruit, the range of method are the 20%-150% of benzalkonium chloride labelled amount.
5, solution stability testing
Precision measure 20 μ l of benzalkonium chloride reference substance solution inject liquid chromatograph, then take preparation, it is specified that under the conditions of place
12 hours, respectively at 0,2,4,6,8,10,12 hour sample introduction, chromatogram is recorded, calculates benzalkonium chloride content (with n-C12H25It takes
For homologue meter) change and calculates RSD.Acceptable standard: benzalkonium chloride content RSD is not more than 2.0%.
As a result it see the table below:
6, detection limit
Benzalkonium chloride reference substance solution is subjected to quantitative dilution, as minimum detection limit (with n- when using signal-to-noise ratio 3:1
C12H25Replace homologue meter), the detection limit concentration of auxiliary material benzalkonium chloride used in this product is 0.37 μ g/ml (7.4ng).
7, quantitative limit
Benzalkonium chloride reference substance solution is subjected to quantitative dilution, as quantitative limit (with n-C when using signal-to-noise ratio 10:112H25It takes
For homologue meter), the quantitative limit concentration of auxiliary material benzalkonium chloride used in this product is 1.47 μ g/ml (29.4ng).
8, durability
Respectively in standard conditions, change that column temperature is 35 DEG C and 45 DEG C, to change flow velocity be 0.8ml/min and 1.2ml/min
Under the conditions of run benzalkonium chloride reference substance solution and preparation test sample, calculate the content of benzalkonium chloride in test sample (with n-C12H25
Replace homologue meter).Acceptable standard are as follows: the separating degree at benzalkonium chloride peak and main ingredient peak should be greater than 1.5 after condition changes, and benzene is pricked
The tailing factor at oronain peak should be less than 1.3, and the RSD of changes of contents should be less than 2.0% after standard conditions and change.
As a result it see the table below:
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (7)
- The method that 1.HPLC method measures benzalkonium chloride content in salmon calcitonin nasal spray in Chinese, which is characterized in that chromatographic column uses ten Eight alkyl silane bonded silica gels are filler, YMC, model: TA12S05-2546WT；The mobile phase A used adds 1.5% triethylamine for 9~11mmol/L ammonium acetate aqueous solution, with glacial acetic acid tune pH to 5.0 ±0.5；Mobile phase B is acetonitrile, with A:B=28~32:72~68 (v/v) isocratic elution.
- 2. the method according to claim 1, wherein the mobile phase A used is 10mmol/L ammonium acetate aqueous solution, The triethylamine for adding 1.5%, with glacial acetic acid tune pH to 5.0 ± 0.5；Mobile phase B is acetonitrile；A:B=30:70 (v/v), it is isocratic to wash It is de-.
- 3. method according to claim 1 or 2, which is characterized in that column temperature is 35-45 DEG C, preferably 40 DEG C.
- 4. method according to claim 1-3, which is characterized in that flow velocity: 0.8-1.2mL/min, preferably 1.0mL/min。
- 5. method according to claim 1-4, which is characterized in that Detection wavelength 262nm.
- 6. method according to claim 1-5, which is characterized in that benzalkonium chloride compares in reference substance solution used Product concentration is 0.8% (v/v).
- 7. the method according to claim 1, wherein including: to take salmon calcitonin nasal spray in Chinese, benzalkonium chloride control Each 20 μ L of product solution injects liquid chromatograph, is detected by chromatographic condition, calculates benzalkonium chloride content by external standard method；Wherein, Directlying adopt salmon calcitonin nasal spray in Chinese is that test sample is detected；Benzalkonium chloride reference substance concentration is in reference substance solution used 0.8% (v/v)；Chromatographic condition: the mobile phase A used adds 1.5% triethylamine for 10mmol/L ammonium acetate aqueous solution, with glacial acetic acid tune pH To 5.0 ± 0.5；Mobile phase B is acetonitrile；A:B=30:70 (v/v), isocratic elution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112014511A (en) * | 2020-09-08 | 2020-12-01 | 湖南华腾医药有限公司 | Method for determining benzalkonium chloride content in disinfectant |
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| CN1401240A (en) * | 2001-08-21 | 2003-03-12 | 味之素株式会社 | Fungicide, composition thereof, use and fungicidal method thereof |
| CN102481301A (en) * | 2009-09-17 | 2012-05-30 | 千寿制药株式会社 | Latanoprost-containing aqueous eye drops and method for inhibiting adsorption of latanoprost to resin |
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