西北药学杂志
西北藥學雜誌
서북약학잡지
Northwest Pharmaceutical Journal
2015年
6期
699-701
,共3页
张小妮%刘雪峰%王嫦鹤%刘海静
張小妮%劉雪峰%王嫦鶴%劉海靜
장소니%류설봉%왕항학%류해정
顶空气相色谱法%盐酸罗匹尼罗原料药%溶剂残留
頂空氣相色譜法%鹽痠囉匹尼囉原料藥%溶劑殘留
정공기상색보법%염산라필니라원료약%용제잔류
headspace GC%ropinirole hydrochloride%residual solvents
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。
目的:建立頂空毛細管氣相色譜法測定鹽痠囉匹尼囉中有機溶劑殘留。方法採用毛細管色譜柱DB‐624(30 m ×320 mm ×1.8μm),載氣為氮氣,流速1.5 mL · min-1,分流比1∶1;FID檢測器,進樣口溫度為200℃,檢測器溫度為250℃;程序升溫,初始溫度35℃,維持5 min ,以10℃· min-1的升溫速率升至240℃,維持5 min;頂空進樣,頂空瓶平衡溫度為100℃,平衡時間30 min。結果甲醇、無水乙醇、二氯甲烷、正己烷、乙痠乙酯、吡啶的線性範圍分彆為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),線性關繫良好。平均迴收率為96.7%,96.1%,95.5%,93.6%,92.7%和92.2%,其RSD分彆為1.6%,1.2%,2.3%,2.7%,3.5%和3.0%。結論所建立的方法準確、簡便、重複性好,可用于鹽痠囉匹尼囉原料藥中6種有機溶劑殘留的測定。
목적:건립정공모세관기상색보법측정염산라필니라중유궤용제잔류。방법채용모세관색보주DB‐624(30 m ×320 mm ×1.8μm),재기위담기,류속1.5 mL · min-1,분류비1∶1;FID검측기,진양구온도위200℃,검측기온도위250℃;정서승온,초시온도35℃,유지5 min ,이10℃· min-1적승온속솔승지240℃,유지5 min;정공진양,정공병평형온도위100℃,평형시간30 min。결과갑순、무수을순、이록갑완、정기완、을산을지、필정적선성범위분별위127.5~1020(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)화5.256~42.05( r=0.9987),선성관계량호。평균회수솔위96.7%,96.1%,95.5%,93.6%,92.7%화92.2%,기RSD분별위1.6%,1.2%,2.3%,2.7%,3.5%화3.0%。결론소건립적방법준학、간편、중복성호,가용우염산라필니라원료약중6충유궤용제잔류적측정。
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 .