摘要
目的建立磺苄西林纳中5种有机溶剂残留量的分离测定方法。方法采用溶液直接进样毛细管气相色谱法，色谱柱为SUPELCOWAX-10的毛细管柱（30m×0．53mm，1．0μm），载气为氮气，以水为溶剂，测定了磺苄西林钠原料药中丙酮、异丙醇、乙醇、醋酸丁酯及正丁醇的残留量.结果5种有机溶剂完全分离，在所考察的浓度范围内线性关系良好，其中丙酮的线性范围在6．3～504．0mg·L^-1（r=0．99985），异丙醇的线性范围在9．76～490．4mg·L^-1（r=0．99995），乙醇的线性范围在7．26～484．0mg·L^-1（r=0．99900），醋酸丁酯的线性范围在8．26～471．2mg·L^-1（r=1．0），正丁醇的线性范围在5．24～508．0mg·L^-1（r=0．99995），各残留溶剂的精密度实验RSD均小于5％，平均回收率在99．1％～101．9％之间。结论誉实验所建立的方法简便、灵敏、准确，可用于磺苄西林钠中有机溶剂残留量的测定。
OBJECTIVE To develop a method for the determination of five residual solvents in sulbenicillin sodium. METHODS The residual solvents including acetone, isopropanol, ethanol, butyl acetate and butanol were quantitatively determined by capillary GC on SUPELCOWAX-10（30 m × 0. 53 mm, 1.0 μ m） column. Water was solvent media, nitrogen was the carrier gas. RESULTS Five residual solvents were compietely separated. The linear range of acetone was 6. 3 - 504. 0 mg· L^-1 （ r = 0. 999 85） ,the linear range of isopropanol was 9.76 - 490. 4 mg· L^-1 （ r = 0. 999 95） , the linear range of ethanol was 7.26 - 484.0 mg· L^-1 （ r = 0. 999 00） , The linear range of butyl acetate was 8.26 - 471.2mg· L^-1（ r = 1.0） and the linear range of butanol was 5.24 - 508.0 mg· L^-1（ r = 0. 999 95）. The RSDs of precision of five residual solvents were less than 5% ,the average recovery rates of the preparation were in the range of 99. 1% - 101.9%. CONCLUSION The method is simple, sensitive, accurate and can be used for the quality control of sulbenieillin sodium.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2008年第21期1654-1656,共3页
Chinese Pharmaceutical Journal
关键词
磺苄西林钠
毛细管气相色谱法
有机溶剂残留量
sulbenicillin sodium
capillary gas chromatography
residual organic solvents
