气相色谱测定消心痛中有机溶剂的残留量

建立了C．C测定消心痛原料药中氯仿、乙酸、乙酸乙酯残留量的方法。采用色谱柱为PEG-20M不锈钢柱(4m×2mm),柱温采用程序升高,起始柱温50℃维持3 min,然后以10℃/min的速率升至180℃维持5 min,再以10℃/min的速率升至280℃维持10 min。FID检测器,检测器温度320℃,进样口温度320℃,氮气为载气,流速50mL/min,氢气流速30 mL/min。空气流速400 mL/min。可使三种有机溶剂完全分离,氯仿在0．0005～0．003 mg/mL的浓度范围内呈良好的线性关系(r=0．9994),回收率为100．3％(RSD＜1．0％)；乙酸乙酯在0．005～0．03 mg/mL的浓度范围内呈良好的线性关系(r=0．9999),回收率为100．5％,(RSD＜1．0％)；乙酸在0．005～0．03 mg/mL的浓度范围内呈良好的线性关系(r=0．9997),回收率为98．7％,(RSD＜1．0％)。

The determination of organic solvent remained in isosorbide dinitrate by GC

A method for the determination of chloroform, acetic acid, acetic ether in isosorbide dinitrate by GC was established. Use PEG-20M(4m x2mm) column, the initial temperature was kept 3 rain at 50℃, and then raised to 180℃ at the rate of 10℃/min and kept 5 min, raised to 280℃ at the same rate and kept 10 min. FID detector, the injection port and detector temperature were 320℃ , N_2 as cartier gas, the flow rate was 50 mL/min, the flow rate of hydrogen and air were 30 ml/min, 400 mL/min respectively. The linear responses ranged from 0.0005～0.003 mg/mL(r= O.9994) of chloroform, 0.005～0.03 mg/mL (r= 0.9999) of acetic ether and 0.005-0.03 mg/mL (r = 0.9997) of acetic acid respectively , the recovery of chloroform, acetic ether, and acetic acid were 100.3% ,100.5% and 98.7% respectively.