Novel Synthesis of Bicalutamide Drug Substance and their Impurities using Imidazolium Type of Ionic Liquid

2012 ◽  
Author(s):  
M. Chand ◽  
Anil Kumar Shukla
2020 ◽  
Vol 18 (1) ◽  
pp. 1020-1029
Author(s):  
Shinkichi Nomura ◽  
Yoshiharu Ito ◽  
Shigehiko Takegami ◽  
Tatsuya Kitade

AbstractAlkyl methanesulfonates are genotoxic impurities that should be limited to an intake of not more than 1.5 µg/day, as regulated by the International Council for Harmonization guideline M7. We herein report a trace analysis of methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS), and isopropyl methanesulfonate (IPMS) in the delgocitinib drug substance using liquid–liquid extraction, with an ionic liquid as the sample-solving medium, and direct injection gas chromatography detected with a flame-ionization detector. The proposed method takes advantage of the fine solubility of ionic liquids toward the drug substance, the good extraction efficiency of alkyl methanesulfonates in liquid–liquid extraction using the Chem Elut cartridge with low-polar organic solvents, and the ability of alkyl methanesulfonates to concentrate in minimum amounts of organic solvent, resulting in excellent sensitivity and selectivity. Specifically, for the preparation of the sample solution, a mixture of 1-butyl-3-methylimidazolium chloride, water, and acetonitrile was used as the sample-solving media, extracted with diethyl ether, and the eluent was concentrated to 1 mL. The method showed good linearity, accuracy, and precision from 1 to 5 ppm, and the limits of detection of MMS, EMS, and IPMS were 0.1, 0.05, and 0.05 ppm, respectively.


2008 ◽  
Vol 19 (2) ◽  
pp. 153-156 ◽  
Author(s):  
Xin Ying Zhang ◽  
Xiao Yan Li ◽  
Xue Sen Fan ◽  
Xia Wang ◽  
Jian Ji Wang ◽  
...  

ChemInform ◽  
2008 ◽  
Vol 39 (26) ◽  
Author(s):  
Xin Ying Zhang ◽  
Xiao Yan Li ◽  
Xue Sen Fan ◽  
Xia Wang ◽  
Jian Ji Wang ◽  
...  

2016 ◽  
Vol 16 (11) ◽  
pp. 6139-6143 ◽  
Author(s):  
Qing Qin ◽  
Tongil Kim ◽  
Xiaochuan Duan ◽  
Jiabiao Lian ◽  
Wenjun Zheng

2008 ◽  
Vol 55 (4) ◽  
pp. 915-918 ◽  
Author(s):  
Rei-Sheu Hou ◽  
Jian-Long Wu ◽  
Hui-Ting Cheng ◽  
You-Teng Xie ◽  
Ling-Ching Chen

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