Ethyl chloroformate as a derivatizing reagent for the gas chromatographic determination of isoniazid and hydrazine in pharmaceutical preparations.

作者: Mohammad Yar KHUHAWAR , Liaquat Ali ZARDARI

DOI: 10.2116/ANALSCI.24.1493

关键词:

摘要: Ethyl chloroformate was examined as a precolumn derivatizing reagent for the gas chromatographic (GC) determination of isoniazid (INH) and hydrazine (HZ). Phenylhydrazine (PHZ) used an internal standard. GC separation carried out on HP-5 column (30 m x 0.32 mm i.d.) with flame ionization detection. The elution at initial temperature 150 degrees C 1 min heating rate 10 C/min up to 250 C, nitrogen flow 4 ml/min split ratio 10:1, v/v. linear calibration ranges INH HZ were observed between 3.5-37.5 3.5-35 microg/ml corresponding detection limits 0.18 0.17 ng reaching detector. method subsequently applied in pharmaceutical preparations, achieving relative standard deviation (RSD) 3.8-5.8%. recovery percentage from syrup 98% RSD 5.2%.

参考文章(20)
Afsaneh Safavi, Mohammad Ali Karimi, Mohammad Reza Hormozi Nezhad, Flow injection determination of isoniazid using N-bromosuccinimide- and N-chlorosuccinimide-luminol chemiluminescence systems Journal of Pharmaceutical and Biomedical Analysis. ,vol. 30, pp. 1499- 1506 ,(2003) , 10.1016/S0731-7085(02)00486-7
Xingwang ZHENG, Zhihui GUO, Zhujun ZHANG, Flow-injection electrogenerated chemiluminescence determination of isoniazid using luminol. Analytical Sciences. ,vol. 17, pp. 1095- 1099 ,(2001) , 10.2116/ANALSCI.17.1095
Acedo-Valenzuela M., Espinosa-Mansilla A., A. Muñoz de la Peña, Cañada-Cañada F., Determination of antitubercular drugs by micellar electrokinetic capillary chromatography (MEKC). Analytical and Bioanalytical Chemistry. ,vol. 374, pp. 432- 436 ,(2002) , 10.1007/S00216-002-1494-5
A. Defilippi, G. Piancone, R. Costa Laia, G. P. Tibaldi, An HPLC screening method for the detection of isonicotinic acid hydrazide in cattle milk Chromatographia. ,vol. 40, pp. 170- 174 ,(1995) , 10.1007/BF02272167
Babu G. GOWDA, Mahaveer B. MELWANKI, Jaldappa SEETHARAMAPPA, Kodagali C. SRINIVASA MURTHY, Spectrophotometric determination of isoniazid in pure and pharmaceutical formulations. Analytical Sciences. ,vol. 18, pp. 839- 841 ,(2002) , 10.2116/ANALSCI.18.839
Bhavika Mohan, Nishi Sharda, Saranjit Singh, Evaluation of the recently reported USP gradient HPLC method for analysis of anti-tuberculosis drugs for its ability to resolve degradation products of rifampicin. Journal of Pharmaceutical and Biomedical Analysis. ,vol. 31, pp. 607- 612 ,(2003) , 10.1016/S0731-7085(02)00715-X
J. Mañes, M.J. Gimeno, J.C. Moltó, G. Font, Fluorimetric determination of hydrazine in isoniazid formulations with 2-hydroxy-1-naphthaldehyde. Journal of Pharmaceutical and Biomedical Analysis. ,vol. 6, pp. 1023- 1027 ,(1988) , 10.1016/0731-7085(88)80128-6
Héctor C. Goicoechea, Alejandro C. Olivieri, Simultaneous determination of rifampicin, isoniazid and pyrazinamide in tablet preparations by multivariate spectrophotometric calibration. Journal of Pharmaceutical and Biomedical Analysis. ,vol. 20, pp. 681- 686 ,(1999) , 10.1016/S0731-7085(99)00072-2
Raviraj M. KULKARNI, Dinesh C. BILEHAL, Sharanappa T. NANDIBEWOOR, Oxidation of isoniazid by quinolinium dichromate in an aqueous acid medium and kinetic determination of isoniazid in pure and pharmaceutical formulations. Analytical Sciences. ,vol. 20, pp. 743- 747 ,(2004) , 10.2116/ANALSCI.20.743
Giampietro Frison, Luciano Tedeschi, Donata Favretto, Aikebaier Reheman, Santo Davide Ferrara, Gas chromatography/mass spectrometry determination of amphetamine-related drugs and ephedrines in plasma, urine and hair samples after derivatization with 2,2,2-trichloroethyl chloroformate Rapid Communications in Mass Spectrometry. ,vol. 19, pp. 919- 927 ,(2005) , 10.1002/RCM.1873