CAJ | 학술논문

目的：建立阿托伐他汀钙原料药中甲醇、丙酮、叔丁醇、正丁醇4种有机溶剂残留量的测定方法。方法：采用顶空毛细管气相色谱法，DB-624石英毛细管柱，检测器为氢火焰离子化检测器，载气为氦气，流速为5.0 mL?min-1，柱温采用程序升温（初始温度40℃，维持3mim，15℃?min-1的速率升温至150℃，维持2 min，再以30℃?min-1的速率降至40℃，维持8 min），进样口温度为180℃，检测器温度为260℃，顶空温度为100℃，平衡时间为30 min，分流比为2∶1，定量环温度为100℃，传输管温度为110℃，进样体积为2 mL。结果：4种有机溶剂在该色谱条件下均能有效分离，峰面积与浓度呈现良好线性关系，精密度、回收率良好。结论：该方法准确、可靠，专属性强，灵敏度高，可用于阿托伐他汀钙原料药中残留溶剂的含量测定。
목적：건립아탁벌타정개원료약중갑순、병동、숙정순、정정순4충유궤용제잔류량적측정방법。방법：채용정공모세관기상색보법，DB-624석영모세관주，검측기위경화염리자화검측기，재기위양기，류속위5.0 mL?min-1，주온채용정서승온（초시온도40℃，유지3mim，15℃?min-1적속솔승온지150℃，유지2 min，재이30℃?min-1적속솔강지40℃，유지8 min），진양구온도위180℃，검측기온도위260℃，정공온도위100℃，평형시간위30 min，분류비위2∶1，정량배온도위100℃，전수관온도위110℃，진양체적위2 mL。결과：4충유궤용제재해색보조건하균능유효분리，봉면적여농도정현량호선성관계，정밀도、회수솔량호。결론：해방법준학、가고，전속성강，령민도고，가용우아탁벌타정개원료약중잔류용제적함량측정。
Objective:To establish a method for the determination of 4 residual solvents including methonal, acetone, tert-buta-nol, n-butanol in atorvastatin calcium raw material.Methods: Headspace capillary GC method was adopted.The determination was performed on DB-624 capillary column at the rate of 5.0 mL?min-1 using helium gas as carrier gas and FID as the detector by temperature programming( initial column temperature of 40 ℃, maintaining for 3 min, then raising to 150 ℃ at a rate of 15 ℃?min-1 ,maintaining for 2 min,and then descending to 40 ℃ at a rate of 30 ℃?min-1 ,maintaining for 8 min).The temperature of the injector was maintaining at 180 ℃and that of detector at 260 ℃.The equilibrium temperature was 100 ℃and equilibrium time was 30 min.The split ratio was 2∶1.The looper temperature was 100 ℃ and the transmission pipe temperature was 110 ℃.The volume of sample was 2 mL.Results:The measured 4 residual solvents were separated completely under given chromatogram sys-tems.The calibration curve of each solvent showed a good linear relationship with precision and recovery.Conclusion:The method is specific, reliable and sensitive, and suitable for the content determination of residual solvents in atorvastatin calcium raw material.