2-Acetoxybenzoic acid - Names and Identifiers
2-Acetoxybenzoic acid - Physico-chemical Properties
Molecular Formula | C9H8O4
|
Molar Mass | 180.16 |
Density | 1.35 |
Melting Point | 134-136 °C (lit.) |
Boling Point | 272.96°C (rough estimate) |
Flash Point | 250 °C |
Water Solubility | 3.3 g/L (20 ºC) |
Solubility | Slightly soluble in water, soluble in ethanol, ether, chloroform, sodium hydroxide solution and sodium carbonate solution. |
Vapor Presure | 0.000124mmHg at 25°C |
Appearance | White powder or crystal |
Color | white |
Exposure Limit | ACGIH: TWA 5 mg/m3NIOSH: TWA 5 mg/m3 |
Merck | 14,851 |
BRN | 779271 |
pKa | 3.5(at 25℃) |
Storage Condition | 2-8°C |
Stability | Stable. Keep dry. Incompatible with strong oxidizing agents, strong bases, strong acids, various other compounds such as iodides, iron salts, quinine salts, etc. |
Sensitive | Easily absorbing moisture |
Refractive Index | 1.4500 (estimate) |
MDL | MFCD00002430 |
Physical and Chemical Properties | White crystalline powder. Odorless, slightly sour. Density 1.35. Melting point 135-138 °c. Stable in dry air, the tide is slowly hydrolyzed into salicylic acid and acetic acid. Slightly soluble in water, soluble in ethanol, ether, chloroform, but also soluble in hydroxide solution or carbonic acid solution, and decomposition. |
Use | Salicylic acid and acetic acid. Slightly soluble in water, soluble in ethanol, ether, chloroform, but also soluble in hydroxide solution or carbonic acid solution, and decomposition. Commonly used antipyretic analgesics. For antipyretic, analgesic, anti-rheumatism, promote the excretion of uric acid in patients with gout, anti-platelet aggregation and biliary ascariasis treatment. |
2-Acetoxybenzoic acid - Risk and Safety
Hazard Symbols | Xn - Harmful
|
Risk Codes | R22 - Harmful if swallowed
R36/37/38 - Irritating to eyes, respiratory system and skin.
|
Safety Description | S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice.
S36/37/39 - Wear suitable protective clothing, gloves and eye/face protection.
|
UN IDs | UN 1851 |
WGK Germany | 1 |
RTECS | VO0700000 |
TSCA | Yes |
HS Code | 29182210 |
Hazard Class | 6.1 |
Packing Group | III |
Toxicity | LD50 orally in mice, rats: 1.1, 1.5 g/kg (Hart) |
2-Acetoxybenzoic acid - Upstream Downstream Industry
2-Acetoxybenzoic acid - Reference
Reference Show more | 1. Wei Liqin Wang Dongsheng Miao small building, etc. Study on anti-inflammatory and analgesic effects of danqiao perfusate [J]. Chinese agricultural Bulletin 2015(2):75-79. 2. Jiang Yatong, Li, Ming, Xue, Gao, Ruiqi. Extraction of aspirin from wastewater by emulsion liquid membrane [J]. Chemical Progress 2018 37(4): 1559-1565. 3. Yu Lili, Fan Tao, Yang Liyan, etc. Study on drug loading and in vitro release of Gelatin Microspheres [J]. Chemical Technology, 2012(06):11-14. 4. Su Yan, Feng Chen, Xin Hui, Li Meng, et al. Optimization of fermentation conditions of Lactobacillus paracasei and evaluation of its fermentation broth [J]. Daily Chemical Industry 2020 v.50;No.334(06):49-54 73. 5. Xiaoyu Yang, Lu Chen, Xiuxiu Xiong, Yun Shu, Dangqin Jin, Yang Zang, Wei Wang, Qin Xu, Xiao-Ya Hu, Molecularly imprinted polymers and PEG double engineered perovskite: an efficient platform for constructing aqueous solution feasible photoelectrochemical se 6. Cao, Weiyi, et al. "Simultaneous Quantification of Aspirin, Its Metabolite Salicylic Acid, and Salvianolic Acid B in Human Plasma Using UPLC-MS/MS." International Journal of Analytical Chemistry 2021 (2021). 7. Mengqiu Lu Haizhen Liang, Pengfei Tu, Yong Jiang. Pharmacodynamic comparison of two different source plants of Murrayae Folium et Cacumen[J]. Journal of Chinese Pharmaceutical Sciences, 2021, 30(1): 49-57.DOI: 10.5246/jcps.2021.01.005 8. Deng, Junlin, et al. "Comparative evaluation of maceration and ultrasonic-assisted extraction of phenolic compounds from fresh olives." Ultrasonics Sonochemistry 37 (2017): 328-334.https://doi.org/10.1016/j.ultsonch.2017.01.023 9. [IF=5.047] Fushi Wang et al."Preparation and functionalization of acetylsalicylic acid loaded chitosan/gelatin membranes from ethanol-based suspensions via electrophoretic deposition."J Mater Chem B. 2018 Apr;6(15):2304-2314 10. [IF=7.46] Xiaoyu Yang et al."Molecularly imprinted polymers and PEG double engineered perovskite: an efficient platform for constructing aqueous solution feasible photoelectrochemical sensor."Sensor Actuat B- Chem. 2020 Feb;304:127321 11. [IF=6.922] Yucui Jiang et al."P2X7R in Mast Cells is a Potential Target for Salicylic Acid and Aspirin in Treatment of Inflammatory Pain."J Inflamm Res. 2021; 14: 2913-2931 12. [IF=6.529] Weiyi Cao et al."Drug-drug interactions between salvianolate injection and aspirin based on their metabolic enzymes."Biomed Pharmacother. 2021 Mar;135:111203 13. [IF=4.142] Wang Huai-Song et al."Anti-cancer adjuvant drug screening via epithelial-mesenchymal transition-related aptamer probe."Anal Bioanal Chem. 2021 Nov;413(28):6951-6962 14. [IF=4.113] Fengyang Li et al."Pretreatment of Indobufen and Aspirin and their Combinations with Clopidogrel or Ticagrelor Alleviates Inflammasome Mediated Pyroptosis Via Inhibiting NF-κB/NLRP3 Pathway in Ischemic Stroke."J Neuroimmune Pharm. 2021 Jan 29 15. [IF=4.073] Qingchi Wang et al."Proteoglycan from Bacillus sp. BS11 Inhibits the Inflammatory Response by Suppressing the MAPK and NF-κB Pathways in Lipopolysaccharide-Induced RAW264.7 Macrophages."Mar Drugs. 2020 Dec;18(12):585 16. [IF=3.24] Jianhua Deng et al."Comparison of analgesic activities of aconitine in different mice pain models."Plos One. 2021 Apr;16(4):e0249276 17. [IF=1.885] Cao Weiyi et al."Simultaneous Quantification of Aspirin Its Metabolite Salicylic Acid, and Salvianolic Acid B in Human Plasma Using UPLC-MS/MS."Int J Anal Chem. 2021;2021:6620868 |
2-Acetoxybenzoic acid - Trait
Authoritative Data Verified Data
- This product is white crystal or crystalline powder; Odorless or microstrip acetic acid odor; In case of moisture, it is slowly hydrolyzed.
- This product is soluble in ethanol, dissolved in three gas methane or ether, slightly soluble in water or anhydrous ether; Dissolved in sodium hydroxide solution or sodium carbonate solution, but decomposed at the same time.
Last Update:2022-01-01 11:59:56
2-Acetoxybenzoic acid - Standard
Authoritative Data Verified Data
This product is 2-(Acetoxy) benzoic acid. The content of C9H804 shall not be less than 99.5% calculated as dry product.
Last Update:2024-01-02 23:10:35
2-Acetoxybenzoic acid - Differential diagnosis
Authoritative Data Verified Data
- take about 0.1g of this product, add 10ml of water, boil, cool, add 1 drop of ferric chloride test solution, which shows the color of Corydalis.
- take about 0.5g of this product, add 10ml of sodium carbonate test solution, boil for 2 minutes, let it cool, and add excess dilute sulfuric acid to precipitate white precipitate, with the odor of acetic acid,
- The infrared absorption spectrum of this product should be consistent with that of the control (Spectrum set 5).
Last Update:2022-01-01 11:59:57
2-Acetoxybenzoic acid - Exam
Authoritative Data Verified Data
clarity of the solution
take 0.50g of this product and dissolve 10ml of sodium carbonate test solution heated to about 45°C. The solution should be clear.
free salicylic acid
new system for clinical use. Take this product about O.lg, precision weighing, put in 10ml children's bottle, add 1% glacial acetic acid in the appropriate amount of fermentation solution, shake to dissolve, and dilute to the scale, shake, as a test solution; take about 10 mg of the salicylic acid reference product, weigh it accurately, put it in a 100ml measuring flask, add an appropriate amount of 1% glacial acetic acid in the fermentation broth to dissolve and dilute it to the scale, shake it well, and take 5ml, in a 50ml measuring flask, dilute to the mark with 1% glacial acetic acid in methanol and shake to a standard solution. Test according to high performance liquid chromatography (General 0512). Silica gel bonded with eighteen alkyl silane was used as the filler; Acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) was used as the mobile phase; The detection wavelength was 303nm. The number of theoretical plates shall not be less than 5000 based on the salicylic acid peak. The separation degree of aspirin peak and salicylic acid peak shall meet the requirements, the chromatogram was recorded. If there is a chromatographic peak in the chromatogram of the test solution that is consistent with the retention time of the salicylic acid peak, the peak area shall be calculated according to the external standard method, and the peak area shall not exceed 0.1%.
easily carbonized
take 0.5g of this product, check according to law (General rule 0842), and control solution (take 0.25 of cobalt chloride solution for color comparison, 0.25 of potassium dichromate solution for color comparison, colorimetric copper sulfate solution 0.40, add water to make 5ml), not deeper.
Related substances
take this product about O.lg, put in a 10ml measuring flask, add an appropriate amount of 1% methanol solution of glacial acetic acid, shake to dissolve and dilute to the scale, shake well, as a test solution; Take 1ml for precision measurement, in a 200ml measuring flask, dilute to the scale with 1% glacial acetic acid in the fermentation broth, shake well, and use as a control solution; Take 1ml of the control solution precisely and put it in a 10ml measuring flask, dilute to the scale with 1% glacial acetic acid in methanol and shake well as a sensitivity solution. Test according to high performance liquid chromatography (General 0512). Silica gel bonded with eighteen alkyl silane as filler; Acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase A, acetonitrile as mobile Phase B, the gradient elution was carried out as follows; The detection wavelength was 276nm. The retention time of the aspirin peak is about 8 minutes, and the separation of the aspirin peak and the salicylic acid peak should meet the requirements. The sample solution, the control solution, the sensitivity solution and the l0ul of the salicylic acid reference solution under the free salicylic acid check item were accurately measured and injected into the liquid chromatograph to record the chromatogram. If there are impurity peaks in the chromatogram of the test solution, the sum of other impurity peak areas except the salicylic acid peak shall not be greater than the main peak area of the control solution (0.5%). The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
loss on drying
take this product, put phosphorus pentoxide as desiccant dryer, under reduced pressure drying at 60°C to constant weight, weight loss should not exceed 0.5% (General 0831).
ignition residue
not more than 0.1% (General rule 0841).
Heavy metals
take l.Og of this product, add 23ml of ethanol to dissolve, add acetate buffer (pH 3.5)2mU to check according to law (General rule 0821 first method), containing heavy metals not more than 10 parts per million.
Last Update:2022-01-01 11:59:58
2-Acetoxybenzoic acid - Content determination
Authoritative Data Verified Data
take this product about 0.4g, precision weighing, add neutral ethanol (phenolphthalein indicator solution neutral) 20ml dissolved, add phenolphthalein indicator solution 3 drops, with sodium hydroxide titration solution (0.lmol/L) titration. Each 1 ml of sodium hydroxide titration solution (0.1 mol/L) corresponds to 18.02mg of C9H804.
Last Update:2022-01-01 11:59:58
2-Acetoxybenzoic acid - Category
Authoritative Data Verified Data
antipyretic analgesic, non-steroidal anti-inflammatory drugs, anti-platelet aggregation drugs.
Last Update:2022-01-01 11:59:59
2-Acetoxybenzoic acid - Storage
Authoritative Data Verified Data
sealed and stored in a dry place.
Last Update:2022-01-01 11:59:59
2-Acetoxybenzoic acid - Aspirin tablets
Authoritative Data Verified Data
This product contains aspirin (C9H304) should be 95.0% to 105.0% of the label.
trait
This product is white tablet.
identification
- take an appropriate amount of fine powder of this product (about 0.lg of aspirin), add 10ml of water, boil, cool, and add 1 drop of ferric chloride solution to show Corydalis color.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
examination
- free salicylic acid was newly used. Take an appropriate amount of fine powder of this product (about 0.5g of aspirin), weigh it accurately, put it in 100ml children's bottle, shake it with 1% methanol solution of glacial acetic acid to dissolve aspirin, and dilute it to the scale, shake well, filter with filter membrane, and take the continued filtrate as the test solution; Take about 15mg of salicylic acid reference substance, weigh it accurately and put it in a 50ml measuring flask, add 1% glacial acetic acid in the fermentation broth to dissolve and dilute to the scale, shake well, take 5ml accurately, put it in a 100ml measuring flask, dilute to the scale with 1% glacial acetic acid in methanol solution, shake well as a control solution. According to the method under the item of aspirin free salicylic acid. If there is a chromatographic peak in the chromatogram of the test solution that is consistent with the retention time of the salicylic acid peak, the peak area shall be calculated according to the external standard method, and 0.3% of the labeled amount of aspirin shall not be exceeded.
- dissolution of this product, according to the dissolution and release determination method (General rule 0931 The first method), with hydrochloric acid solution (dilute hydrochloric acid 24ml and water to 1000ml, obtained) 500ml(50mg specification) or 1000ml(0.lg, 0.3g, 0.5g specifications) for the dissolution of the medium, the speed is 100 rpm, according to the law, after 30 minutes, take 10ml solution filtration, take the filtrate as the test solution; Take the aspirin reference substance, precision weighing, add 1% methanol solution of glacial acetic acid to dissolve and dilute to make 0.08mg(50mg, 0.lg specification), 0.24mg(0.3g specification) or 0.4mg(0.5g specification) solution, as aspirin reference solution; Take salicylic acid reference, precision weighing, add 1% glacial acetic acid in methanol solution dissolved and diluted to make each 1 ml containing 0.01mg(50mg, 0.1G specification), 0.03mg(0.3g specification) or 0.05mg(0.5g specification) solution, as salicylic acid control solution. According to the chromatographic conditions under the content determination item, the sample solution, the reference substance solution of AstraZeneca and the reference substance solution of salicylic acid were accurately measured and respectively injected into the human liquid chromatograph, and the chromatograms were recorded. The content of aspirin and salicylic acid in each tablet is calculated by peak area according to external standard method, and the dissolved amount of each tablet is obtained by multiplying the content of salicylic acid by 1.304 and adding the content of aspirin. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others shall be in accordance with the relevant provisions under the item of tablets (General rule 0101).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system applicability test using eighteen alkyl silane bonded silica as filler; Using acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase; the detection wavelength was 276nm. The number of theoretical plates shall not be less than 3000 calculated by aspirin peak, and the separation degree of aspirin peak and salicylic acid peak shall meet the requirements.
- determination Method: Take 20 tablets of this product, accurately weigh and fully grind, accurately weigh an appropriate amount of fine powder (about 10 mg of aspirin), and put it in a 100ml measuring flask, dissolve aspirin by strong shaking with 1% methanol solution of glacial acetic acid, dilute to the scale with 1% methanol solution of glacial acetic acid, shake well, filter through the filter, and take the continued filtrate as the test solution, lOul was accurately measured and injected into human liquid chromatograph, and the chromatogram was recorded, A solution of 1% glacial acetic acid in methanol was added, dissolved and quantitatively diluted by shaking to obtain a content of about 0.lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as aspirin.
specification
(l)50mg (2)0.lg (3)0.3g (4)0.5g
storage
sealed and stored in a dry place.
Last Update:2022-01-01 12:00:00
2-Acetoxybenzoic acid - Aspirin enteric-coated tablets
Authoritative Data Verified Data
This product contains aspirin (C9H804) should be 93.0% ~ 107.0% of the label amount.
trait
This product is an enteric coated tablet, White after removing the coating.
identification
- take an appropriate amount of fine powder of this product (about 0.1g of aspirin), add 10ml of water, boil, cool, and add 1 Drop of iron trihydrate test solution to show Pansy color.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
examination
- free salicylic acid was newly used. Take an appropriate amount of fine powder (approximately equivalent to aspirin O.lg ), weigh precisely, put it in a 100ml measuring flask, add 1% methanol solution of glacial acetic acid to shake to dissolve aspirin, dilute to the scale, shake well, filter through the filter, take the continued filtrate as the test solution; Take about 15mg of the salicylic acid reference, weigh it accurately, put it in a 50ml measuring flask, dissolve it with 1% methanol solution of glacial acetic acid, dilute it to the scale, shake it well, take 5ml precision, 100ml flask, diluted with methanol solution of glacial acetic acid to the scale, shake, as a reference solution. According to the method under the item of aspirin free salicylic acid. If there is a chromatographic peak in the chromatogram of the test solution that is consistent with the retention time of the salicylic acid peak, the peak area shall be calculated according to the external standard method, and 1.5% of the labeled amount of aspirin shall not be exceeded.
- dissolution acid dissolution amount of this product, according to the dissolution and release determination method (General rule 0931 first method 1), with 0.lmol /L hydrochloric acid solution 600ml(25mg, 40mg, 50mg specifications) or 750ml(100mg, 300mg specifications) as the dissolution medium, speed of 100 rpm, according to the law of operation, after 2 hours, take 10ml of the solution, filter, and take the filtrate as the test solution; Take the aspirin reference substance, precision weigh, add 1% glacial acetic acid methanol solution dissolved and diluted to make each lml containing 4.25ug(25mg specification), 7ug(40mg specification), 8.25ug(50mg specification), 13ug(100mg specification) 40UG (300mg specification) of the solution, as a control solution. Measured according to the method under the item of content determination. Calculate the amount of aspirin dissolved in each tablet, the limit should be less than 10% of the labeled amount of aspirin.
- elution amount in buffer solution under the acid elution amount check item, 0.2mol/L Sodium Stannate solution at 37°C (25mg, 40mg, 50mg specifications) was further added. Or 250ml(l00mg, 300mg specification), mix well, adjust the pH value of the solution with 2mol/L hydrochloric acid solution or 2mol/L sodium hydroxide solution to 6.8±0.05, continue to dissolve for 45 minutes, take 10ml of the solution, filter, take the filtrate as the test solution; Take the appropriate amount of aspirin reference by precision weighing, add 1% glacial acetic acid methanol solution to dissolve and dilute to make each lml containing 22ug(25mg specification), 35ug(40mg specification), 44ug(50mg specification), 72ug(lOOmg specification), 0.2mg (300mg specification) solution, as aspirin control solution; Another salicylic acid control, precision weighing, add 1% glacial acetic acid methanol solution dissolved and diluted into 1 ml containing 1.7ug ( 25mg specification), 2.6ug(40mg specification), 3.4ug(50mg specification), 5.5ug(100mg specification) 16UG (300mg specification) solution, as salicylic acid control solution. According to the chromatographic conditions under the content determination item, the sample solution, the aspirin reference solution and the salicylic acid reference solution are respectively injected into the liquid chromatograph, and the chromatograms are recorded. The content of aspirin and salicylic acid in each tablet was calculated according to the external standard method, and the salicylic acid content was multiplied by 1.304, and the amount of aspirin was added to obtain the release amount of each buffer. The limit is 70% of the labeled amount and shall be in accordance with the provisions.
- others shall be in accordance with the relevant provisions under the item of tablets (General rule 0101).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica as filler, acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase; the detection wavelength was 276mn. The number of theoretical plates shall not be less than 3000 calculated by aspirin peak, and the separation degree of aspirin peak and salicylic acid peak shall meet the requirements.
- determination Method: Take 20 tablets of this product, accurately weigh, fully grind, accurately weigh an appropriate amount (about 10mg equivalent to aspirin), and put it in a 100ml measuring flask, add 1% methanol solution of glacial acetic acid and shake strongly to dissolve aspirin and dilute it to the scale, filter the filter, take the filtrate as the test solution, and take 10ul injection liquid chromatograph for precision measurement, record the chromatogram; Take another aspirin reference substance, precision weighing, add 1% glacial acetic acid in methanol solution dissolved and quantitatively diluted to make each 1 ml containing 0.lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as aspirin.
specification
(l)25mg (2)40mg (3)50mg (4) lOOmg(5)300mg
storage
sealed and stored in a dry place.
Last Update:2022-01-01 12:00:01
2-Acetoxybenzoic acid - Aspirin enteric-coated capsules
Authoritative Data Verified Data
This product contains aspirin (C9H804) should be 93.0% ~ 107.0% of the label amount.
trait
The contents of this product are white granules or enteric coated pellets, which appear white after removing the coating.
identification
- take an appropriate amount of the content of this product (about 0.lg of aspirin), add 10ml of water, boil, cool, and add 1 drop of ferric chloride solution to show the color of Corydalis.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
examination
- free salicylic acid was newly used. Take an appropriate amount of fine powder (about 0.1g of aspirin) under the content determination item, weigh it accurately, put it in a 100ml measuring flask, and shake with 1% methanol solution of glacial acetic acid to dissolve aspirin and dilute it to the scale, shake well, filter the filter membrane, and take the continued filtrate as the test solution; Take about 10mg of the salicylic acid reference substance, weigh it accurately and put it in a 100ml measuring flask, add 1% methylated solution of glacial acetic acid to dissolve and dilute to the scale, shake well, take 1ml, put it in a 10ml measuring flask, dilute it to the scale with 1% methanol solution of glacial acetic acid, shake well as a control solution. The assay was performed according to the method under the item of Aselin free salicylic acid. If there is a chromatographic peak in the chromatogram of the test solution that is consistent with the retention time of the salicylic acid peak, the peak area shall be calculated according to the external standard method, and 1.0% of the labeled amount of aspirin shall not be exceeded.
- dissolution of this product, according to the dissolution and release determination method (General rule 0931 first method 1 ) , with 0.1 mol/L hydrochloric acid solution 750ml as the dissolution medium, the speed is 100 rpm, according to the law, after 2 hours, take the appropriate amount of solution, filtering, the filtrate was taken as the test solution (1). In the above acid solution, immediately add 0.2mol/L sodium phosphate solution at 37°C, mix well, adjust the pH value of the solution with 2mol/L hydrochloric acid solution or 2mol/L sodium hydroxide solution to 6.8±0.05, the dissolution was continued for 45 minutes, an appropriate amount of the solution was taken, filtered, and the continued filtrate was taken as the test solution (2). Take aspirin reference substance, precision weighing, add 1% glacial acetic acid methanol solution dissolved and diluted into 0.06mg(0.075g specification), 0.08mg (0.lg specification), 0.12mg (0.15g specification) of the solution, as aspirin control solution (1); Precision take aspirin control solution (l)15ml, 100ml flask, dilute to the scale with 1% glacial acetic acid methanol solution, shake well, as aspirin reference solution (2); Take another salicylic acid reference, add 1% glacial acetic acid in methanol solution dissolved and diluted to make each 1 ml containing 7.5ug(0.075g specification) 10ug(O.lg specification), 15ug (0.15g specification) solution, as salicylic acid control solution. According to the chromatographic conditions under the content determination item, take the sample solution (1), (2) and aspirin reference solution (1), (2) and salicylic acid reference solution 10 u1, respectively, injection of human liquid chromatography, record chromatogram. Test Solution (1) with aspirin reference solution (2) as the control, according to the external standard method to calculate the peak area of each particle in the dissolution of acid, the limit should be less than 10% of the labeled amount of aspirin; test Solution (2) with the reference solution (1) and the salicylic acid reference solution as the control, the content of aspirin and salicylic acid in each particle is calculated by the peak area according to the external standard method, the salicylic acid content is multiplied by 1.304 and added to the amount of aspirin dissolved to give the amount of each tablet dissolved in the buffer. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others should comply with the relevant provisions under the capsule (General 0103).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system applicability test using eighteen alkyl silane bonded silica as filler; Using acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase; the detection wavelength was 276nm. The number of theoretical plates shall not be less than 3000 calculated by aspirin peak, and the separation degree of aspirin peak and salicylic acid peak shall meet the requirements.
- the contents under the item of difference in loading amount were measured, ground finely, and weighed accurately. Take an appropriate amount (approximately equal to 10 mg of aspirin) and place it in a 100ml measuring flask, add 1% methanol solution of glacial acetic acid and shake strongly to dissolve aspirin and dilute to the scale, filter through the filter, take the filtrate as the test solution, and inject 10ul into the liquid chromatograph with precision, record the chromatogram; Take another aspirin reference substance, precisely weigh, add 1% glacial acetic acid in methanol solution to dissolve and quantitatively dilute to make about 0 per 1 ml. lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as aspirin.
specification
(l)0.075g (2)0.lg (3)0.15g
storage
sealed and stored in a dry place.
Last Update:2022-01-01 12:00:02
2-Acetoxybenzoic acid - Aspirin effervescent tablets
Authoritative Data Verified Data
This product contains aspirin (C9H804) should be 90.0% ~ 110.0% of the label amount.
trait
This product is white or light yellow, one-sided scattered small yellow spots.
identification
- take an appropriate amount of fine powder of this product (about 0.lg of aspirin), add 10ml of water, boil, cool, and add 1 drop of ferric chloride solution to show Corydalis color.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
examination
- free salicylic acid was newly used. Precision weighing this product fine powder appropriate amount (approximately equivalent to assilin O.lg), put it in a 100ml measuring flask, add 1% methanol solution of glacial acetic acid to shake to dissolve aspirin, dilute to the scale, shake well, filter through a filter, and take the continued filtrate as a test solution; take about 15mg of salicylic acid reference product, weigh it accurately, put it in 50ml measuring flask, dissolve it with 1% methanol solution of glacial acetic acid and dilute it to the standard, shake it well, take 1 ml and put it in 10ml measuring flask, dilute to the mark with 1% glacial acetic acid in fermentation broth, shake well, as a control solution; Determine according to the method under aspirin free salicylic acid. If there are chromatographic peaks with the same retention time as the salicylic acid peak in the chromatogram of the test solution, the peak area shall be calculated according to the external standard method, and 3.0% of the amount of aspirin standard 75 shall not be passed.
- In addition to friability, it shall comply with the relevant provisions under the item of tablets (General rule 0101).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica as filler, acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase; the detection wavelength was 276nm. The number of theoretical plates shall not be less than 3000 calculated by aspirin peak, and the degree of separation between aspirin peak and salicylic acid peak shall meet the requirements.
- determination of 10 tablets of this product, precision weighing, fully fine, precision weighing fine powder (about 10 mg equivalent to aspirin), put in a 100ml measuring flask, add 1% methanol solution of glacial acetic acid to be dissolved by strong shaking, dilute to the scale with 1% methanol solution of glacial acetic acid, shake well, filter through the filter, and take the continued filtrate as the test solution, take 10u1 injection of human liquid chromatograph for accurate measurement, record chromatogram; Take aspirin reference substance for accurate weighing, A solution of 1% glacial acetic acid in methanol was added to dissolve and quantitatively dilute with shaking to make about O per 1 ml. lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as aspirin.
specification
(1)0.lg (2)0.5g
storage
sealed and stored in a dry place.
Last Update:2022-01-01 12:00:03
2-Acetoxybenzoic acid - Aspirin suppositories
Authoritative Data Verified Data
This product contains aspirin (C9H804) should be 90.0% ~ 110.0% of the label amount.
trait
This product is milky white or yellowish suppository.
identification
take an appropriate amount of this product (about 0.6g of aspirin), add 20ml of ethanol, dissolve aspirin at a slight temperature, cool in an ice bath for 5 minutes, stir and filter continuously, the filtrate was evaporated to dryness on a water bath, and the residue was tested according to items (1) and (2) of identification under the item of aspirin, showing the same results.
examination
- free salicylic acid was newly used. Accurately measure 5ml of the stock solution of the test product under the content determination item, put it in a 10ml measuring flask, dilute it to the scale with 1% methanol solution of glacial acetic acid, and shake it up to be used as the test solution; take about 15mg of salicylic acid reference, weigh it accurately, put it in 50ml measuring flask, add 1% methanol solution of glacial acetic acid to dissolve and dilute it to the scale, shake it well, and take 1 ml of it accurately, in a 10ml measuring flask, dilute to the mark with 1% glacial acetic acid in methanol, and shake to a standard solution. According to the method under the item of aspirin free salicylic acid. If there is a chromatographic peak in the chromatogram of the test solution that is consistent with the retention time of the salicylic acid peak, the peak area shall be calculated according to the external standard method, and 3.0% of the labeled amount of aspirin shall not be exceeded.
- others should comply with the relevant provisions under suppository (General rule 0107).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica as filler, acetonitrile-tetrahydrofuran-glacial acetic acid-water (20:5:5:70) as mobile phase; the detection wavelength was 276nm. The number of theoretical plates shall not be less than 3000 calculated by aspirin peak, and the separation degree of aspirin peak and salicylic acid peak shall meet the requirements.
- determination Method: Take 5 grains of this product, weigh them precisely, put them in a small beaker, melt them at a slight temperature in a water bath at 40-50°C, and cool them under constant stirring, precision weighing an appropriate amount (approximately equivalent to aspirin O.lg ), put it in a 50ml measuring flask, add an appropriate amount of 1% methanol solution of glacial acetic acid, and fully shake in a water bath at 40-50°C to dissolve azelastin and let it cool, dilute to the scale with 1% methanol solution of glacial acetic acid, shake well, cool in an ice bath for 1 hour, remove, rapidly filter, and take the continued filtrate as a sample stock solution. Precisely take 5ml stock solution of the test sample, put it in a 100ml measuring flask, dilute it to the scale with 1% methanol solution of fermented ice and acid, shake it well, and then inject lOul into the liquid chromatograph, record the chromatogram; Take another aspirin reference substance, weigh it precisely, add 1% glacial acetic acid in methanol solution, shake it to dissolve and quantitatively dilute it to make it contain about O per 1 ml. lmg solution, the same method for determination. According to the external standard method to calculate the peak area, that is.
category
Same as aspirin.
specification
(l)0.1g (2)0.15g (3 )0.3g (4 )0.45g(5)0.5g
storage
sealed and stored in a cool and dry place.
Last Update:2022-01-01 12:00:04
2-Acetoxybenzoic acid - Reference Information
introduction | aspirin, also known as acetylsalicylic acid, belongs to non-steroidal anti-inflammatory drugs and was first used for anti-inflammatory analgesia. Later, scientists discovered that aspirin has the effect of preventing platelet aggregation to achieve antithrombotic effect. With the deepening of research on aspirin, many new uses have been discovered. For example, aspirin can reduce the mortality of myocardial infarction and stroke, and can also reduce the risk of colorectal cancer. |
pharmacological effects | acetylsalicylic acid (aspirin) is a traditional antipyretic and analgesic, and has the effect of anti-platelet aggregation. Acetylsalicylic acid (aspirin) has anti-thrombotic properties in the body and can reduce the formation of obstructive thrombosis in peripheral arteries. Inhibits the release of platelets and the release of endogenous ADP, 5-HT, etc. Therefore, the second phase aggregation of platelets is inhibited without inhibiting their first phase aggregation. The mechanism of action of acetylsalicylic acid (aspirin) is to acetylate the cyclooxygenase of platelets, thereby inhibiting the formation of peroxides in the ring, and the production of TXA2 is also reduced. It also acetylates platelet membrane proteins and inhibits platelet membrane enzymes, which also helps to inhibit platelet function. Because cyclooxygenase is inhibited, it affects the synthesis of PGI2 on the blood vessel wall; it can also inhibit the enzyme of platelet TXA2 synthesis. For example, in large doses, the production of TXA2 and PGI2 is affected. It is suitable for ischemic heart disease. After coronary artery surgery (PTCA) and coronary artery bypass grafting, it can prevent transient cerebral ischemia, stroke, and myocardial infarction, and reduce the incidence of arrhythmia. |
indications | acetylsalicylic acid, also known as aspirin, has an inhibitory effect on platelet aggregation, can prevent thrombosis, and is clinically used to prevent temporary ischemic attack, myocardial infarction, arterial thrombosis and atherosclerosis. In addition, it can also treat biliary ascariasis. |
clinical application | acetylsalicylic acid is also called aspirin as an antiplatelet aggregation drug. Antithrombotic: This product has an inhibitory effect on platelet aggregation and can prevent thrombosis. It is clinically used to prevent transient ischemic attack, myocardial infarction, atrial fibrillation, artificial heart valve, arteriovenous fistula or other post-operative thrombosis. It can also be used to treat unstable angina. |
pharmacokinetics | oral bioavailability is 68±3%, and blood drug concentration peaks at 2~3 h. Plasma protein binding rate was 50% ~ 90%. Renal clearance rate was 9.3±1.1 mL/(min kg). T1/220 min; Salicylate T1/23~5 h, T1/215~30 h in large dose. The effective anti-inflammatory concentration in plasma is 150~300 μg/mL, and the toxic concentration is greater than 200 μg/mL. The 90% is excreted by the kidney in the binding type and the 10% in the free type. After urine alkalization, free drug excretion increased 3~5 times. |
preparation | vitamin c (ascorbic acid) is a vitamin drug with certain acidity, which does not have the problems of equipment corrosion and environmental pollution, and has a wide range of reaction properties to chemical reagents. its application in the synthesis of aspirin is reported: when 6.3g salicylic acid, 13.5mL acetic anhydride, two vitamin C tablets were reacted at 65 ℃ for 20 min with 90.1% aspirin yield and 15 rain at 75 ℃ with 92.6% yield. |
chemical properties | this product is a white crystal, m.p.138 ~ 140 ℃, insoluble in water, soluble in alcohol, ether, etc. |
use | acetylsalicylic acid is the raw material for preparing rodenticide intermediate 4-hydroxycoumarin. Yang acid and acetic acid. Slightly soluble in water, soluble in ethanol, ether, chloroform, and also soluble in alkaline hydroxide solution or carbonic acid solution, and decomposed at the same time. Commonly used antipyretic analgesics. It is used for antipyretic, analgesic, anti-rheumatic, promoting the excretion of uric acid in gout patients, anti-platelet aggregation and biliary ascariasis treatment. used to manufacture outdoor and strong light-irradiated structural parts and equipment parts, such as automobile body, agricultural machinery parts, electric meters and lamp shades, road markings, etc. antipyretic analgesics, used for fever, pain and rheumatoid Arthritis, etc. is the earliest, most extensive and most common antipyretic and analgesic antirheumatic drugs. It has many pharmacological effects such as antipyretic, analgesic, anti-inflammatory, anti-wind and anti-platelet aggregation. It has rapid efficacy and positive efficacy. Overdose is easy to diagnose and handle, and allergic reactions rarely occur. It is often used for colds and fever, headache, neuralgia, joint pain, muscle pain, rheumatic fever, acute internal wet arthritis, rheumatoid arthritis and toothache. Acetylsalicylic acid is a variety listed in the "National Essential Drug List" and is also an intermediate of other drugs. Verification of manganese. Organic synthesis. Acetylsalicylic acid prevents the production of prostate cord by inhibiting cyclooxygenase (cyclooxygenase, prostaglandin H synthase), especially for COX-1 isoform. Its antithrombotic effect is due to the inhibition of COX-1, which plays a role in coagulation and platelet aggregation in platelets. |
production method | salicylic acid is acetylated by adding acetic anhydride (0.7889 times of the total amount of salicylic acid) in the reaction tank, adding 2/3 amount of salicylic acid, stirring and heating, and reacting at 81-82 ℃ for 40-60min. The temperature was cooled to 81-82 ℃ for 2h. After checking that the free salicylic acid is qualified, the temperature is lowered to 13 ℃, crystallization is precipitated, filtered, washed and dried with water, and air dried at 65-70 ℃ to obtain acetylsalicylic acid. the preparation method is to first put salicylic acid and acetic anhydride into a three-mouth bottle and stir, the reaction temperature does not exceed 60 ℃, after about 1h, the reaction is over, poured into ice water, crystallization is precipitated, filtered and dried to obtain the product. |
category | toxic substances |
toxicity classification | highly toxic |
acute toxicity | oral-rat LD50: 200 mg/kg; Oral-hour LD50: 250 mg/kg |
flammability hazard characteristics | open flame flammability; stimulating gas |
storage and transportation characteristics | warehouse ventilation and low temperature drying; Separate storage with oxidant and food additives |
fire extinguishing agent | mist water, foam, carbon dioxide, sand. |
occupational standard | TWA 5 mg/m3 |
NIST chemical information | The information is provided by: webbook.nist.gov (external link) |
EPA chemical information | The information is provided by: ofmpub.epa.gov (external link) |
toxic substance data | information provided by: pubchem.ncbi.nlm.nih.gov provided (external link) |
Last Update:2024-09-05 10:16:05