Determination of residual amines used in bulk drug synthesis by pre-column derivatization with 3,5-dinitrobenzoyl chloride and high-performance liquid chromatography

Morley, James A.; Elrod, Lee; Linton, Cathie L.; Shaffer, Dean I.; Krogh, Suzanne

doi:10.1016/s0021-9673(96)01058-8

Cited by 7 publications

(3 citation statements)

References 11 publications

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“…18,31 Derivatization is a promising approach, which can reduce the volatility and polarity of the analytes, and hence improve the selectivity and sensitivity of aliphatic amines in chromatographic analysis. Several derivatizing reagents, such as 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, 32,33 2,4-dinitrophenylhydrazine, 34 3,5-dinitrobenzoy, 35 9-uorenylmethylchloroformate 36 and OPA, 19 have been utilized to derivatize aliphatic amines offline. As a popular derivatizing reagent, OPA is derivatized offline with primary amines to form highly uorescent substances.…”

Section: Evaluation Of Online Derivatizationmentioning

confidence: 99%

Quantitative analysis of aliphatic amines in urban aerosols based on online derivatization and high performance liquid chromatography

Huang

Deng

Zhuang

et al. 2016

Environ. Sci.: Processes Impacts

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A method combining online derivatization with high performance liquid chromatography/fluorescence detection was developed for the determination of seven aliphatic amines (ethanolamine, methylamine, ethylamine, propylamine, butylamine, pentylamine and hexylamine) in urban aerosols. The collected amines were online derivatized with o-phthalaldehyde to form highly fluorescent sulfonatoisoindole derivatives. The derivatives were completely separated in 13 min through gradient elution and detected by fluorescence detection at an excitation wavelength of 334 nm and an emission wavelength of 443 nm. Under the optimized conditions, the relative standard derivations (RSDs) of all detected amines were 0.02-2.03% and 1.04-1.52% for the retention time and peak area, respectively. Excellent linearity was achieved for each analyte, ranging from 5 μg L(-1) to 1000 μg L(-1) (R(2) > 0.99). The detection limits for all analytes were below 1.1 μg L(-1). The proposed method was used to analyze aliphatic amines in 35 samples of urban PM2.5 collected in Shanghai and was found to be suitable for the determination of particulate aliphatic amines at ng m(-3) levels in ambient air. Based on our measurements, ethanolamine and methylamine were the most abundant species on average in Shanghai during dry and wet seasons. The highest concentration was 15.3 ng m(-3) for ethanolamine and 13.2 ng m(-3) for methylamine.

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Section: Evaluation Of Online Derivatizationmentioning

confidence: 99%

Quantitative analysis of aliphatic amines in urban aerosols based on online derivatization and high performance liquid chromatography

Huang

Deng

Zhuang

et al. 2016

Environ. Sci.: Processes Impacts

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“…Separation and identification of piperazine by thin -layer chromatography [23,24] . The HPLC for piperazine estimation [25][26][27][28][29][30][31][32][33][40][41][42]. GC method for the determination piperazine in pharmaceutical drug substances, chicken and pig tissues [34,35,42] .…”

Section: Chromatographic Methodsmentioning

confidence: 99%

A Review on Analytical Methods for Piperazine Determination

Al-Neaimy

Saeed

Shehab

2022

NTU-JPS

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Piperazine compounds mediate their anthelmintic action by generally paralyzing parasites, allowing the host body to easily remove or expel the invading organism. It is an anthelmintic drug in human as well as in veterinary medicine. This review article represent the various analytical methods which has been reported for estimation of piperazine. The colorimetric , spectrophotometric techniques and chromatographic methods like HPLC and RP HPLC, GC, LC-MS, LC-MS/MS and another methods were reported.

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“…Different stereoselective chromatographic modes and techniques are used for these purposes. Some examples include determination of enantiomeric purity of (3S)-(-)-tert-butoxycarbonylamino) pyrrolidine by HPLC on a-AGP CSP after derivatization to 3,5-dinitrobenzoyl derivative under Schotten-Baumann reaction, 106 chiral purity of levodopa and methyl dopa by a chiral ligand-exchange chromatography with N,N-dimethyl-L-phenylalanine and Cu(II) 107 enantioseparation of several pharmaceutical intermediates on Chiralcel OD and Chiralpak AD columns with hexane mobile phase modified by ethanol or 2-propanol, 108 or determination of enantiomers of 3-tert-butylamino-1,2-propanediol, an intermediate for the industrial synthesis of b-blocker, (S)-timolol. 109 Table 9 lists other examples of such applications of direct mode stereoselective HPLC.…”

Section: Determination Of Drug Enantiomers In Body Fluidsmentioning

confidence: 99%