中国实验方剂学杂志
中國實驗方劑學雜誌
중국실험방제학잡지
CHINESE JOURNAL OF EXPERIMENTAL TRADITIONAL MEDICAL FORMULAE
2013年
23期
146-150
,共5页
李德斌%黄志芳%刘云华%刘玉红%陈燕%易进海
李德斌%黃誌芳%劉雲華%劉玉紅%陳燕%易進海
리덕빈%황지방%류운화%류옥홍%진연%역진해
炮天雄%酯型生物碱%质量标准%薄层色谱%高效液相色谱
砲天雄%酯型生物堿%質量標準%薄層色譜%高效液相色譜
포천웅%지형생물감%질량표준%박층색보%고효액상색보
processed Aconitum carmichaeli%ester-type alkaloids%quality standard%thin-layer chromatography%high performance liquid chromatography
目的:建立炮天雄的质量标准.方法:采用薄层色谱法对苯甲酰新乌头原碱进行定性研究;采用高效液相色谱方法,选用Eclipse XDB-C18色谱柱(4.6 mm ×250 mm,5μm),柱温35℃,流动相A为0.1 mol·L-1醋酸铵溶液(每1 000 mL加冰醋酸0.5 mL),B为四氢呋喃-乙腈(15∶25),梯度洗脱,体积流量1 mL·min-1,检测波长235 nm.结果:炮天雄中水分为10.1%~12.3%;定性鉴别专属性强;苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱分别在0.049 4 ~1.976,0.023 32 ~0.932 8,0.049 95 ~1.998,0.024 46 ~0.978 56,0.024 91 ~0.996 48,0.022 02 ~0.880 8 μg进样量呈良好线性关系,r均为0.999 9;平均回收率分别为98.79%,100.66%,97.06%,97.91%,103.58%,102.77%; RSD分别为1.90%,2.23%,1.91%,1.96%,1.08%,2.19%.结论:该方法操作简便,结果准确,可作为炮天雄的质量控制方法.
目的:建立砲天雄的質量標準.方法:採用薄層色譜法對苯甲酰新烏頭原堿進行定性研究;採用高效液相色譜方法,選用Eclipse XDB-C18色譜柱(4.6 mm ×250 mm,5μm),柱溫35℃,流動相A為0.1 mol·L-1醋痠銨溶液(每1 000 mL加冰醋痠0.5 mL),B為四氫呋喃-乙腈(15∶25),梯度洗脫,體積流量1 mL·min-1,檢測波長235 nm.結果:砲天雄中水分為10.1%~12.3%;定性鑒彆專屬性彊;苯甲酰新烏頭原堿、苯甲酰烏頭原堿、苯甲酰次烏頭原堿、新烏頭堿、次烏頭堿和烏頭堿分彆在0.049 4 ~1.976,0.023 32 ~0.932 8,0.049 95 ~1.998,0.024 46 ~0.978 56,0.024 91 ~0.996 48,0.022 02 ~0.880 8 μg進樣量呈良好線性關繫,r均為0.999 9;平均迴收率分彆為98.79%,100.66%,97.06%,97.91%,103.58%,102.77%; RSD分彆為1.90%,2.23%,1.91%,1.96%,1.08%,2.19%.結論:該方法操作簡便,結果準確,可作為砲天雄的質量控製方法.
목적:건립포천웅적질량표준.방법:채용박층색보법대분갑선신오두원감진행정성연구;채용고효액상색보방법,선용Eclipse XDB-C18색보주(4.6 mm ×250 mm,5μm),주온35℃,류동상A위0.1 mol·L-1작산안용액(매1 000 mL가빙작산0.5 mL),B위사경부남-을정(15∶25),제도세탈,체적류량1 mL·min-1,검측파장235 nm.결과:포천웅중수분위10.1%~12.3%;정성감별전속성강;분갑선신오두원감、분갑선오두원감、분갑선차오두원감、신오두감、차오두감화오두감분별재0.049 4 ~1.976,0.023 32 ~0.932 8,0.049 95 ~1.998,0.024 46 ~0.978 56,0.024 91 ~0.996 48,0.022 02 ~0.880 8 μg진양량정량호선성관계,r균위0.999 9;평균회수솔분별위98.79%,100.66%,97.06%,97.91%,103.58%,102.77%; RSD분별위1.90%,2.23%,1.91%,1.96%,1.08%,2.19%.결론:해방법조작간편,결과준학,가작위포천웅적질량공제방법.