CAJ | 학술논문

目的：采用气相顶空色谱法测定马来酸氟吡汀原料药中的甲醇、乙醇和异丙醇3种有机溶剂的残留量。方法：采用DB-624(30 m ×0.53 mm,3.0μm)毛细管色谱柱,载气为氮气,程序升温。 FID检测器,温度为250℃。进样口温度为200℃。按外标法测定溶剂残留量。结果：甲醇,乙醇和异丙醇分别在2.182~152.74(r=0.9991),3.546~248.22(r=0.9998)和4.082~285.74μg·ml-1(r =0.9997)范围内,线性关系良好；平均回收率分别为97.7%(RSD =1.5%),99.0%(RSD =1.1%),98.8%(RSD=1.1%)(n=5)。结论：本方法简便、准确,灵敏度高,适用于马来酸氟吡汀原料药中有机溶剂残留量的检测。
목적：채용기상정공색보법측정마래산불필정원료약중적갑순、을순화이병순3충유궤용제적잔류량。방법：채용DB-624(30 m ×0.53 mm,3.0μm)모세관색보주,재기위담기,정서승온。 FID검측기,온도위250℃。진양구온도위200℃。안외표법측정용제잔류량。결과：갑순,을순화이병순분별재2.182~152.74(r=0.9991),3.546~248.22(r=0.9998)화4.082~285.74μg·ml-1(r =0.9997)범위내,선성관계량호；평균회수솔분별위97.7%(RSD =1.5%),99.0%(RSD =1.1%),98.8%(RSD=1.1%)(n=5)。결론：본방법간편、준학,령민도고,괄용우마래산불필정원료약중유궤용제잔류량적검측。
Objective:To determine the content of methanol, alcohol and isopropanol in flupirtine maleat by headspace gas chro-matography. Methods:The capillary gas chromatography with programming temperature was established with an FID detector and a DB-624(30 m × 0. 53 mm,3. 0 μm) capillary column. The temperature of the injector and the detector was 200℃ and 250℃, respec-tively. The residual organic solvents were determined by an external standard method. Results: Methanol, alcohol and isopropanol showed good linearity within the range of 2. 182~152. 74(r=0. 999 1), 3. 546-248. 22(r=0. 9998)and 4. 082-285. 74 μg·ml-1(r=0. 999 7) with the average recovery of 97. 7%(RSD=1. 5%),99. 0%(RSD=1. 1%)and 98. 8%(RSD=1. 1%)(n=5), respec-tively. Conclusion:The method is simple, sensitive and accurate, and can be used in the residual solvents detection for flupirtine mal-eat.