中国药事
中國藥事
중국약사
CHINESE PHARMACEUTICAL AFFAIRS
2014年
9期
1014-1017
,共4页
氢溴酸高乌甲素%乙醇%乙酸乙酯%三氯甲烷%苯%有机溶剂残留%顶空毛细管气相色谱
氫溴痠高烏甲素%乙醇%乙痠乙酯%三氯甲烷%苯%有機溶劑殘留%頂空毛細管氣相色譜
경추산고오갑소%을순%을산을지%삼록갑완%분%유궤용제잔류%정공모세관기상색보
lappaconitehydrobrom%ethanol%ethylacetate%chloroform%benzene%residual solvent%headspace gas chromatography
目的：建立测定氢溴酸高乌甲素中4种有机溶剂残留量的顶空毛细管气相色谱方法。方法采用DB-624毛细管柱(30 m ×0.53 mm,3μm),程序升温,起始柱温40℃,维持7 min,以25℃·min-1的速率升至200℃,维持1 min；进样口温度：200℃；FID 检测器,检测器温度：250℃；进样方式：顶空进样,平衡温度：80℃,平衡时间：30 min；载气为N2；以DMF为溶剂对氢溴酸高乌甲素中乙醇、乙酸乙酯、三氯甲烷和苯的残留量进行测定。结果4种有机溶剂分离度良好,乙醇、乙酸乙酯、三氯甲烷和苯浓度分别在129.2~1033μg·mL-1(r=0.999)、120.5~964.2μg·mL-1(r=0.999)、3.32~26.5μg·mL-1(r=0.998)、0.14~1.13μg·mL-1(r=0.997)范围内线性关系良好；平均回收率(n=9)分别为97.4%、97.4%、96.8%、98.1%,RSD 分别为1.3%、2.0%、1.7%、3.1%。结论本文建立的顶空毛细管气相色谱法,经方法学验证可用于氢溴酸高乌甲素中有机溶剂残留量的测定,可作为该药质量标准修订的参考。
目的：建立測定氫溴痠高烏甲素中4種有機溶劑殘留量的頂空毛細管氣相色譜方法。方法採用DB-624毛細管柱(30 m ×0.53 mm,3μm),程序升溫,起始柱溫40℃,維持7 min,以25℃·min-1的速率升至200℃,維持1 min；進樣口溫度：200℃；FID 檢測器,檢測器溫度：250℃；進樣方式：頂空進樣,平衡溫度：80℃,平衡時間：30 min；載氣為N2；以DMF為溶劑對氫溴痠高烏甲素中乙醇、乙痠乙酯、三氯甲烷和苯的殘留量進行測定。結果4種有機溶劑分離度良好,乙醇、乙痠乙酯、三氯甲烷和苯濃度分彆在129.2~1033μg·mL-1(r=0.999)、120.5~964.2μg·mL-1(r=0.999)、3.32~26.5μg·mL-1(r=0.998)、0.14~1.13μg·mL-1(r=0.997)範圍內線性關繫良好；平均迴收率(n=9)分彆為97.4%、97.4%、96.8%、98.1%,RSD 分彆為1.3%、2.0%、1.7%、3.1%。結論本文建立的頂空毛細管氣相色譜法,經方法學驗證可用于氫溴痠高烏甲素中有機溶劑殘留量的測定,可作為該藥質量標準脩訂的參攷。
목적：건립측정경추산고오갑소중4충유궤용제잔류량적정공모세관기상색보방법。방법채용DB-624모세관주(30 m ×0.53 mm,3μm),정서승온,기시주온40℃,유지7 min,이25℃·min-1적속솔승지200℃,유지1 min；진양구온도：200℃；FID 검측기,검측기온도：250℃；진양방식：정공진양,평형온도：80℃,평형시간：30 min；재기위N2；이DMF위용제대경추산고오갑소중을순、을산을지、삼록갑완화분적잔류량진행측정。결과4충유궤용제분리도량호,을순、을산을지、삼록갑완화분농도분별재129.2~1033μg·mL-1(r=0.999)、120.5~964.2μg·mL-1(r=0.999)、3.32~26.5μg·mL-1(r=0.998)、0.14~1.13μg·mL-1(r=0.997)범위내선성관계량호；평균회수솔(n=9)분별위97.4%、97.4%、96.8%、98.1%,RSD 분별위1.3%、2.0%、1.7%、3.1%。결론본문건립적정공모세관기상색보법,경방법학험증가용우경추산고오갑소중유궤용제잔류량적측정,가작위해약질량표준수정적삼고。
Objective To establish a headspace gas chromatography method for determination of four residual solvents in lappaconite hydrobrom.Methods The residual solvents in lappaconite hydrobrom were separated on the DB-624 column (30 m × 0.53 mm,3μm)with an FID detector.The injector temperature and the detector temperature were set at 200 ℃and 250 ℃.The initial temperature was 40 ℃and kept for 7 min, the temperature was then raised to 200 ℃ at the rate of 25 ℃· min-1 and lasted 1 min.The containers of headspace injector were in equilibrium for 30 min at 80 ℃.The DMF was used as the solvent to determine the four residual solvents in lappaconite hydrobrom.Results Four residual solvents were completely separated. Good linearities of the four solvents were obtained within the range of 129.2-1033μg·mL-1 (r=0.999), 120.5-964· 2 μg.mL-1 (r=0.999),3.32-26.5 μg · mL-1 (r=0.998),0.14-1.13μg· mL-1 (r=0.997).The average recoveries (n=9 )of ethanol,ethyl acetate,chloroform,benzene were 97.4%, 97.4%,96.8%,98.1% and the RSDs were 1.3%,2.0%,1.7%,3.1%,respectively.Conclusion The established method was in accordance with the requirements of the methodology validation which can be used for the determination of four residual solvents in lappaconite hydrobrom,and can provide a reference for the drug quality standard revision.
