摘要
目的建立测定头孢唑兰原料药中甲醇、乙醇、丙酮、二氯甲烷和乙酸乙酯5种有机溶剂残留量的方法。方法采用顶空气相色谱法。检测器为氢火焰离子化检测器(FID);色谱柱为Agilent DB-624毛细管柱(30m×0.32mm,1.8μm);溶剂为二甲基亚砜;进样口温度为220℃;检测器温度为250℃;分流比为20∶1;用程序升温;氮气为载气;氢气和空气为燃气;顶空平衡温度90℃;平衡时间30min;进样体积1mL。结果 5种有机溶剂在建立的色谱条件下均能完全分离,分离度均大于1.5,理论塔板数均大于10 000;在考察质量浓度范围内线性关系良好(甲醇、乙醇、丙酮、二氯甲烷和乙酸乙酯的r值分别为0.998 3,0.997 7,0.998 5,0.995 5和0.997 7);定量限分别为29.850,30.225,3.960,15.100和3.675μg·mL^(-1);检测限分别为7.460,7.560,1.190,4.530和1.100μg·mL^(-1);重复性RSD值均小于2.5%(n=6);平均回收率范围为98.00%~101.44%;混合对照品溶液在10h内稳定性良好。结论该方法操作简便、灵敏、结果准确、可靠,可用于头孢唑兰原料药中有机溶剂残留量的控制。
Objective To establish a headspace gas chromatography method for the determination of methanol,ethanol,acetone,methylene chloride and ethyl acetate residual solvents in cefozopran. Methods The experiment was carried out by headspace gas chromatography with a hydrogen flame ionization detector (FID) and an Agilent DB-624 capillary column (30 m×0.32 mm,1.8 μm).The sample was dissolved in DMSO solvent.The temperature of Inlet was 220 ℃ and the temperature of detector was 250 ℃.The split ratio was set to 20∶1.Program temperature was used in the whole process,and N 2 was used as carrier gas,H 2 and air were used as burn gas.The headspace balance temperature was 90 ℃,and the balance time was 30 min.In such conditions,the sample was injected 1 mL each time. Results 5 kinds of organic solvents were completely separated under the established chromatographic conditions, R 〉1.5, N 〉10 000;the linear relationships were good in the mass concentration ranges (methanol r = 0.998 3, ethanol r = 0.997 7, acetone r = 0.998 5, dichloromethane r = 0.995 5, ethyl acetate r =0.997 7);the limit of quantification was 29.850,30.225,3.960,15.100 and 3.675 μg·mL -1 ,respectively;the limit of detection were 7.460,7.560,1.190,4.530 and 1.100 μg·mL -1 ,respectively.The average recovery rates were between 98.44%-101.44%.The mixed reference substances kept stable within 10 h. Conclusion The method is simple,sensitive,accurate and reliable,and can be used for the control of residual solvents in cefozopran.
作者
易梦娟
许军
刘燕华
王晨
田太平
李豫园
YI Mengjuan;XU Jun;LIU Yanhua;WANG Chen;TIAN Taiping;LI Yuyuan(College of Pharmacy,Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China)
出处
《西北药学杂志》
CAS
2018年第6期739-742,共4页
Northwest Pharmaceutical Journal
基金
江西中医药大学研究生校级创新专项资金项目(编号:JZYC16S30)
关键词
头孢唑兰
顶空气相色谱法
原料药
有机溶剂
残留量
cefozopran;headspace gas chromatography;active pharmaceutical ingredient;organic solvent;residual