TRACE LEVEL QUANTIFICATION OF CYPIONYL CHLORIDE IN TESTOSTERONE CYPIONATE BY PRE COLUMN DERIVATIZATION WITH 2-BUTANOL BY GAS CHROMATOGRAPHY WITH ELECTRON IMPACT IONIZATION DETECTORAbstract
The author has been proposed the precolumn derivatization method for the trace level quantification of cypionyl chloride in testosterone cypionate, it maybe potential impurity in the testosterone cypionate, it has to quantify in the testosterone drug Substance. The method development of cypionyl chloride has been started with gas chromatography with FID detector. The detection of cypionyl chloride was very poor and detection was less even for derivatization with 2-butanol in GC-FID detector. The GC-MS Electron impact ionization detector with derivatization by 2-butanol was developed and validated for trace level quantification of cypionyl chloride in Testosterone cypionate. The LOQ of this method was 1.7 ppm and the LOD was 0.6 ppm. The validation parameters were done against the ICH Q2 R1 guidelines. The precision, linearity, accuracy and solution stability was met the ICH Q2 R1 guidelines.
N. Rajana *, P. Madhavan, J. M. Babu, K. Basavaiah and D. R. Devi
Scientist in Analytical Research and Development, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories Ltd., Miyapur, Hyderabad, Telangana, India.
16 October, 2017
21 December, 2017
25 December, 2017
01 July, 2018