Bromination of Acridine

2018 ◽  
Vol 71 (4) ◽  
pp. 285
Author(s):  
Graham S. Chandler ◽  
Wolfgang H. F. Sasse

The quantitative determination of the products of bromination of acridine in concentrated sulfuric acid and glacial acetic acid is described. In both cases, the only monobromo products were the 2- and 4-substituted compounds. With sulfuric acid, the 4-isomer predominates whereas in acetic acid, the 2-isomer is predominant. This work expands substantially on the tiny amount of previous work on halogenation of dibenzo-annelated pyridines.

1959 ◽  
Vol 5 (6) ◽  
pp. 609-614 ◽  
Author(s):  
Armand J Courchaine ◽  
William H Miller ◽  
Donald B Stein

Abstract A rapid procedure for the determination of both free and total cholesterol in serum is described. The color development is extremely rapid, and once fully developed the color remains stable for several hours. The heat of reaction produced by the combination of concentrated sulfuric acid, phosphoricacid, and glacial acetic acid is apparently responsible for the rapid color development. The stable ferric chloride reagent containingphosphoric acid appears to be the contributing factor to the stability of the color. The results obtained with this procedure compare favorably with those obtained with saponification methods.


2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC


2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.


1999 ◽  
Vol 365 (4) ◽  
pp. 310-313
Author(s):  
B. Hammouti ◽  
H. Oudda ◽  
A. El Maslout ◽  
A. Benayada

1968 ◽  
Vol 46 (23) ◽  
pp. 3643-3648 ◽  
Author(s):  
Réal Laliberté ◽  
Hilda Warwick ◽  
Georges Médawar

Some derivatives of α-cyano tétrahydro benzothiazoline-Δ2α-acetic acid and their intermediates are described. The lack of reactivity of this class of compounds and products of treatment with concentrated sulfuric acid have been studied. Assignment of configuration was based on infrared and ultraviolet spectroscopic evidence.


1982 ◽  
Vol 65 (4) ◽  
pp. 927-929
Author(s):  
Brian R Bennett ◽  
Gregory S Grimes

Abstract Chlorophacinone and diphacinone are extracted at the 0.005% level from grain or paraffinized baits with glacial acetic acid. The target concentration is 0.01 mg/mL. The filtered supernate is chromatographed on a Partisil PXS ODS10/25 liquid chromatography column with premixed and degassed glacial acetic acid-tetrahydrofuran-water (14 + 2 + 9) and detected at 288 nm. The concentration is calculated by using an external standard. The recovery from spiked samples averaged 96.6% for both analytes. The response is linear from 0.001 to 0.040 mg/mL. The coefficient of variation of within-day replicates ranged from 1.1 to 2.5%.


1978 ◽  
Vol 61 (1) ◽  
pp. 129-135
Author(s):  
Yukio Saito ◽  
Hiroshi Sekita ◽  
Mitsuharu Takeda ◽  
Mitsuru Uchiyama

Abstract An analytical method was developed for determining benzo (a) pyrene in foods, suitable for routine use. The method consists of 4 cleanup steps: (1) alkali cleavage of sample, (2) preliminary silica gel column chromatography, (3) selective extraction with concentrated sulfuric acid, and (4) further silica gel column chromatography. Recoveries of benzo- (a) pyrene added to 50 g (or 10 g) food at levels of 0.4 ppb (or 2 ppb) ranged from 70% for short-necked clam and mackerel to 85% for chicken meat. The sulfuric acid extraction step affords a simple method for isolating benzo (a)- pyrene from various kinds of interfering substances which could not be separated by existing methods.


1965 ◽  
Vol 48 (4) ◽  
pp. 771-774
Author(s):  
D P Johnson ◽  
H A Stansbury

Abstract A method has been developed for detecting residues of carbaryl (1-naphthyl methylcarbamate) as well as its hydrolysis product, 1-naphthol, in dead bees. The method is based on extraction of the bees with benzene, followed by a cleanup involving liquid partitioning and chromatography on Florisil. The quantitative determination involves hydrolysis of carbaryl to 1-naphthol and coupling of the latter with p-nitrobenzenediazonium fluoborate in acetic acid to form a yellow substance. For separate analysis, free 1-naphthol is separated from methylene chloride into a basic aqueous solution. The sensitivity of the method is about 0.1 ppm; recoveries averaged 85.6 ± 6.6% for 1- naphthol and 83.8 ± 2.7% for carbaryl.


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