中国执业药师
中國執業藥師
중국집업약사
CHINA LICENSED PHARMACIST
2015年
7期
9-11,15
,共4页
比卡鲁胺%残留溶剂%N,N-二甲基甲酰胺%气相色谱法
比卡魯胺%殘留溶劑%N,N-二甲基甲酰胺%氣相色譜法
비잡로알%잔류용제%N,N-이갑기갑선알%기상색보법
Bicalutamide%Residual Solvents%DMF%Gas Chromatography
目的：建立直接进样气相色谱法检测比卡鲁胺原料药中有机残留溶剂N，N-二甲基甲酰胺的方法。方法：色谱柱为Agilent INNOWAX弹性石英毛细管柱（30.0 m×0.25 mm，0.25μm）；进样口温度：200℃；氢火焰离子化检测器（FID）温度：250℃；柱温：程序升温，初始温度60℃，以10℃/min的速率升至200℃，维持3 min；载气：氮气；流速：1.0 mL/min；直接进样，进样体积：1.0μL；以N-甲基吡咯烷酮为溶解介质。结果：被测溶剂能良好分离，N，N-二甲基甲酰胺峰面积与浓度均呈良好的线性关系。结论：该法精密度良好，回收率均较为理想，适用于比卡鲁胺原料药中残留溶剂N，N-二甲基甲酰胺的测定。
目的：建立直接進樣氣相色譜法檢測比卡魯胺原料藥中有機殘留溶劑N，N-二甲基甲酰胺的方法。方法：色譜柱為Agilent INNOWAX彈性石英毛細管柱（30.0 m×0.25 mm，0.25μm）；進樣口溫度：200℃；氫火燄離子化檢測器（FID）溫度：250℃；柱溫：程序升溫，初始溫度60℃，以10℃/min的速率升至200℃，維持3 min；載氣：氮氣；流速：1.0 mL/min；直接進樣，進樣體積：1.0μL；以N-甲基吡咯烷酮為溶解介質。結果：被測溶劑能良好分離，N，N-二甲基甲酰胺峰麵積與濃度均呈良好的線性關繫。結論：該法精密度良好，迴收率均較為理想，適用于比卡魯胺原料藥中殘留溶劑N，N-二甲基甲酰胺的測定。
목적：건립직접진양기상색보법검측비잡로알원료약중유궤잔류용제N，N-이갑기갑선알적방법。방법：색보주위Agilent INNOWAX탄성석영모세관주（30.0 m×0.25 mm，0.25μm）；진양구온도：200℃；경화염리자화검측기（FID）온도：250℃；주온：정서승온，초시온도60℃，이10℃/min적속솔승지200℃，유지3 min；재기：담기；류속：1.0 mL/min；직접진양，진양체적：1.0μL；이N-갑기필각완동위용해개질。결과：피측용제능량호분리，N，N-이갑기갑선알봉면적여농도균정량호적선성관계。결론：해법정밀도량호，회수솔균교위이상，괄용우비잡로알원료약중잔류용제N，N-이갑기갑선알적측정。
Objective:To establish a method for the determination of residual solvent dimethylformamide (DMF)in the drug substance of bicalutamide by gas chromatography(GC).Methods:The residual solvent DMF in the drug substance was determined by GC equipped with FID detector and linked with Agilent INNOWAX capillary column(30.0 m×0.25 mm,0.25μm). The inlet temperature was at 200 ℃and the FID detector temperature was at 250 ℃. The column temperature rose by program, the initial temperature was at 60 ℃and raised to 200 ℃with a rate of 10 ℃/min and maintained for 3 min. The carrier gas was nitrogen and the flow rate of carrier gas was 1.0 mL/min. The injection volume was 1.0μL. The dissolved medium used was methylpyrrolidone(NMP). Results:The solvent DMF could be completely separated in chromatogram and there was a good linear relationship between the peak area and concentration of DMF within a certain range.Conclusion:The method is accurate and reliable with a good recovery. It can be applied in the determination of residual solvent DMF in the drug substance of bicalutamide.
