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Lab. quiz chromatography
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3) LITERATURE REVIEW Aceclofenac • Aceclofenac is official in IP & BP but not official in USP. • Official methods: Sr. No. Title Description Ref. No. 1. Estimation of Aceclofenac and re-leated substances. (IP 2010) • Liquid chromatographic sys-tem: • Column: a stainless steel col-umn 25 cm x 4.6 mm packed with spherical end-capped octadecylsilane bonded to porous silica (5µm), with a pore size of 10 µm and carbon loading of 19 per cent • Mobile phase: A. a 0.112 per cent w/v solu-tion of orthophosphoric acid adjusted to pH 7.0 using a 4.2 per cent solution of sodium hydroxide, B. 1 volume of water and 9 volumes of acetonitrile • Flow rate: 1 ml per minute • UV detection: 275 nm • Injection volume:10 µL 23 2. Assay of aceclofenac (IP 2010) • Weigh accurately about 0.3 g and dissolve in 40 ml of me-thanol. Titrate with 0.1 M so-dium hydroxide. • Determine the end point potentiometrically. Carry out a blank titration. • 1ml of 0.1 M sodium hydroxide is equivalent to 0.03542 g of C16H13Cl2NO4 23 3. Estimation of aceclofenac and re-leated substances. (BP 2007) • Liquid chromatographic sys-tem: • Column: - size: 1= 0.25 m, 0 = 4.6 mm; - stationary phase: spherical end capped octadecylsilyl silica gel for chromatography R (5 µm) with a pore size of 10 nm and a carbon loading of 19 per cent; - temperature: 40 ºC. • Mobile phase: - mobile phase A: 1.12 gil solu-tion of phosphoric acid R adjusted to pH 7.0 using a 42 gil solution of sodium hydroxide R; - mobile phase B: water R, aceto nitrile R (1:9 VIV); • Flow rate: 1.... ... middle of paper ... ... valida-tion of HPLC method for the determination of pregabalin in capsule. • Column: Hypersil BDS, C8, 150×4.6mm,5µm • Mobile phase: phosphate buf-fer pH 6.9 and acetonitrile in the ratio of 95:05 • Flow rate: 1 ml/min • LOQ: 0.6mg/l 41 4. Analytical RP-HPLC method for development and validation of prega-balin and methylcobala-mine in combined cap-sule formulation. • Column: (250 × 4.6mm, 5mcg/ml) • Flow rate: 1ml/min • Uv detection: 210nm • Mobile phase: Ammonium dihydrogen-o-phosphate (buf-fer 6.0), acetonitrile and me-thanol in the ratio of 75:15:10. • Linearity range: 3200-4800 mcg/ml (pregaba-lin) 16-24 mcg/ml (methylcoba-lamine) • LOD value: 47.93 mcg/ml (pregabalin) 1.33 mcg/ml (methylcobala-mine) • LOQ value: 145 mcg/ml (pregabalin) 4.05 mcg/ml (methylcobola-mine) 42
The mixture was poured through a weight filter paper and Sucrose washed with a 5ml of dichloromethane. The resulting solid was left in a breaker to dry for one week, to be measured. Left it in the drawer to dry out for a week and weighted it to find the sucrose amount recovered amount.
We were then to make a base solution of 0.7 M NaOH. In order to standardize
I decided to experiment with pHs within the range pH 2 to pH7, as I
The HPLC method used was 20 μL of sample at 25°C through an RI detector for 15 minutes. The mobile phase was .0001M Sulfuric acid at .6ml/min with a column temperature of 60°C.
This done by boiling pills in hydroiodic acid and red phosphorus, red phosphorus comes from
increase the PH up to the optimum and then decrease the PH as the PH
Base being Baking Soda, or Sodium Bicarbonate, and the acid being Vinegar, or Acetic Acid for a control. I measured 10 ml. of Vinegar, dumped that into a two inch high glass jar, and wrote down the pH level. Then I measured o...
Aceclofenac is a non-steroidal anti-inflammatory drug, widely used in the management of osteoarthritis, rheumatoid arthritis and ankylosing spondylitis. Usual therapeutic dose is 100 mg twice daily and half life is 3-4 hrs; thus it is necessary to be administered frequently in order to maintain the desired concentration. Therefore, Aceclofenac is an ideal candidate for sustained release formulation, resulting in more reproducible drug absorption and reducing the risk of local irritations.5
What would you give to rid yourself of acne? What would you do? The bane of every adolescent’s existence, these red spots develop to some degree in 85% of the population between ages 12 and 25 (Lamberg). Teenagers wake up every morning, look at the mirror, and sigh at the acne on their faces and often other places on their bodies. They dread these awful things that are absolutely ugly. They get desperate and eventually, if the acne grows worse than ever before, they resort to Accutane. Accutane, also known as isotretinoin, is a medication for acne. However, despite isotretinoin’s helpfulness in controlling acne that is unresponsive to other treatments, this medication should not be used because of its harmful physical side effects, its association with psychiatric adverse effects, and its effects on reproduction.
Remove the extra solvent on a steam bath under a hood while flushing the flask with N2 gas, leaving the crude extract. Weigh extract.
From looking at the results I can conclude that when the pH was 3 and
Griswold, Norman E. "Standardizing a Sodium Hydroxide Solution." General Chemistry For Engineering And Science I. Mason: Cengage Learning, 2012. 141-48. Print. Signature Lab Ser.
Add 15mL of 6N sulfuric acid to a 125mL Erlenmeyer flask containing 105mL of deionized water (preparing approximately 0.75N sulfuric acid). Obtain a sample of the unknown. Weight the vial and contents accurately on an analytical balance. Handle the vial with a small strip of paper to reduce the risk of error (due to added weight). Pour about half of the sample into a clean dry 200mL Erlenmeyer flask and weight again. Use the remaining half of the sample to get a second weight of around 0.6g-0.7g. Make sure the vial is capped on every weight taken.
Each tablet was placed on pre-weighed container, and then they were weighted by using the digital balanceafter making sure that any extra drops of water was uninvolved and the container was completely dry and clean. This step was repeated for each tablet to determine the exact swelling percentage through the following formula