顶空气相色谱法测定头孢唑肟钠中残留有机溶剂

Determination of the residual organic volatile solvents in ceftizoxime sodium by head-space GC

目的：测定头孢唑肟钠中残留有机溶剂乙醇、二氯甲烷、丙酮和醋酸乙酯的含量。方法：采用顶空气相色谱法，氢火焰离子化检测器，以水为溶剂，醋酸丙酯为内标，在6％氰丙基苯-94％二甲基硅氧烷（0．32mm×30mm，1．8μm）毛细管色谱柱上，以柱温40℃维持7min后，以15℃／min升温至100℃，维持20min，各组分达到基线分离。结果：乙醇、丙酮、二氯甲烷和醋酸乙酯测定线性范围分别为20～200、20～200、12—120和20～200μg/ml，相关系数（r）分别为0．9978、0．9961、0．9926和0．9995，平均回收率分别为98．3％、102．7％、100．2％和99．2％（n=9）。结论：本方法简便、灵敏度高、结果准确，适用于头孢唑肟钠中有机溶剂的残留量测定。

OBJECTIVE To determine the residual organic volatile solvents（ dichloromethane,ethyl alcohol,acetone and ethyl acetate ）. METHODS Head - space gas chromatography, the GC was equipped a flame - ionization detector. A （ 0.32 mm × 30 mm, 1.8 μm） chromatographic column was coated with 6% cyanopropylpolysiloxane and 94% dimethylpolysiloxane stationary phase. The cartier was nitrogen. The column temperature was 40 ℃ for 7 min, then the temperature slowly was raised to 100 ℃ by the rate of 15 ℃/rain and sustained 20 min. Under this condition, dissolved water ,four organic residues and the internal standard ethyl acetate were separated thoroughly. RESULTS Ethyl alcohol, acetone, dichloromethane and ethyl acetate were respectively 20 - 200,20 - 200,12 - 120 and 20 - 200 μg/ml , the correlation was 0. 997 8,0. 996 1,0. 992 6 and 0. 999 5, the recovery was 98. 3% ,102.7% ,100.2% and 99.2% separately. CONCLUSION This method is sensitive, accurate and easy to be operated, and can be used for the determination of the residual organic volatile solvents in ceftizoxime sodium.