顶空气相色谱法测定盐酸罗匹尼罗原料药的溶剂残留

摘要

目的：建立顶空毛细管气相色谱法测定盐酸罗匹尼罗中有机溶剂残留。方法采用毛细管色谱柱DB‐624（30 m ×320 mm ×1．8μm），载气为氮气，流速1．5 mL · min－1，分流比1∶1；FID检测器，进样口温度为200℃，检测器温度为250℃；程序升温，初始温度35℃，维持5 min ，以10℃· min－1的升温速率升至240℃，维持5 min；顶空进样，顶空瓶平衡温度为100℃，平衡时间30 min。结果甲醇、无水乙醇、二氯甲烷、正己烷、乙酸乙酯、吡啶的线性范围分别为127．5～1020（r＝0．9987），75．09～600．7（ r＝0．9967），15．03～120．3（ r＝0．9997），7．212～57．70（ r＝0．9994），125．6～1005（ r＝0．9992）和5．256～42．05（ r＝0．9987），线性关系良好。平均回收率为96．7％，96．1％，95．5％，93．6％，92．7％和92．2％，其RSD分别为1．6％，1．2％，2．3％，2．7％，3．5％和3．0％。结论所建立的方法准确、简便、重复性好，可用于盐酸罗匹尼罗原料药中6种有机溶剂残留的测定。%Objective To establish a headspace capillary GC method for the determination of residual solvents in ropinirole hydro‐chloride .Methods The experimental condition was as follows :ADB‐624 capillary column(30 m × 320 mm × 1 .8 μm) was used , N2 was used as the carrier gas at a flow rate of 1 .5 mL · min-1 ,and split rate was 1∶1 ;The injector temperature was 200 ℃ and the FID detector was 250 ℃ ;The oven temperature was initially held at 35 ℃ for 5 min and then programmed to 240 ℃ at 10 ℃ · min-1 and held for 5 min;The headspace sampling was used at heated temperature 100 ℃ for 30 min .Results The linear ranges of meth‐anol ,ethanol ,methylene ,chloride ,n‐hexane ,ethylacetate ,pyridine were 127 .5‐1 020(r=0 .999 17) ,75 .09‐600 .7(r=0 .996 7) , 15 .03‐120 .3(r=0 .999 7) ,7 .212‐57 .70(r=0 .999 4) ,125 .6‐1 005(r=0 .999 2)and 5 .256‐42 .05(r=0 .998 7) ,respectively .The average recoveries were 96 .7% ,96 .1% ,95 .5% ,93 .6% ,92 .7% and 92 .2% ,respectively ,and the RSD were 1 .6% ,1 .2% , 2 .3% ,2 .7% ,3 .5% and 3 .0% ,respectively .Conclusion The method is accurate ,and repeatable .It can be applied for the deter‐mination of 6 residual solvents in ropinirole hydrochloride .