河北医学
河北醫學
하북의학
HEBEI MEDICINE
2014年
4期
537-540
,共4页
青娥丸%液质联用%高效液相色谱
青娥汍%液質聯用%高效液相色譜
청아환%액질련용%고효액상색보
Qing'e pill%LC-MS/MS%HPLC
目的:通过液质联用( LC-MS/MS)与高效液相色谱( HPLC)测定青娥丸中药效成分-松脂醇二葡萄糖苷、补骨脂素和异补骨脂素的含量比对,为其质量控制提供方法参考。方法:采用Kromasil C18色谱柱,以甲醇-0.1%甲酸为流动相进行梯度洗脱,使用多反应监测( MRM)模式,监测离子对为m/z 700.5→m/z 235.4(松脂醇二葡萄糖苷)、m/z 187.1→m/z 131.1(补骨脂素和异补骨脂素)进行LC-MS/MS法同时测定,与药典HPLC法分别测定的结果进行对比分析,比较二者的差异性。结果:3种成分LC-MS/MS法测定的方法回收率分别为99.08%、98.95%和98.56%,RSD分别为1.33%、1.43%和1.27%。结论:LC-MS/MS法同时测定青娥丸中的药效成分,与药典HPLC法相比具有简便、灵敏、准确等特点,适用于青娥丸的含量测定。
目的:通過液質聯用( LC-MS/MS)與高效液相色譜( HPLC)測定青娥汍中藥效成分-鬆脂醇二葡萄糖苷、補骨脂素和異補骨脂素的含量比對,為其質量控製提供方法參攷。方法:採用Kromasil C18色譜柱,以甲醇-0.1%甲痠為流動相進行梯度洗脫,使用多反應鑑測( MRM)模式,鑑測離子對為m/z 700.5→m/z 235.4(鬆脂醇二葡萄糖苷)、m/z 187.1→m/z 131.1(補骨脂素和異補骨脂素)進行LC-MS/MS法同時測定,與藥典HPLC法分彆測定的結果進行對比分析,比較二者的差異性。結果:3種成分LC-MS/MS法測定的方法迴收率分彆為99.08%、98.95%和98.56%,RSD分彆為1.33%、1.43%和1.27%。結論:LC-MS/MS法同時測定青娥汍中的藥效成分,與藥典HPLC法相比具有簡便、靈敏、準確等特點,適用于青娥汍的含量測定。
목적:통과액질련용( LC-MS/MS)여고효액상색보( HPLC)측정청아환중약효성분-송지순이포도당감、보골지소화이보골지소적함량비대,위기질량공제제공방법삼고。방법:채용Kromasil C18색보주,이갑순-0.1%갑산위류동상진행제도세탈,사용다반응감측( MRM)모식,감측리자대위m/z 700.5→m/z 235.4(송지순이포도당감)、m/z 187.1→m/z 131.1(보골지소화이보골지소)진행LC-MS/MS법동시측정,여약전HPLC법분별측정적결과진행대비분석,비교이자적차이성。결과:3충성분LC-MS/MS법측정적방법회수솔분별위99.08%、98.95%화98.56%,RSD분별위1.33%、1.43%화1.27%。결론:LC-MS/MS법동시측정청아환중적약효성분,여약전HPLC법상비구유간편、령민、준학등특점,괄용우청아환적함량측정。
Objective:To compare the determination of effective components -pinoresinol diglucoside , psoralen and isopsoralen in Qing'e pill by LC-MS/MS and HPLC, to provide reference method for its quality control.Method:A Kromasil C18 column was used with the mobile phase of methanol-0.1%formic acid for gradient elution.ESI was applied with MRM mode .The transitions of m/z 700.5→m/z 235.4 ( pinoresinol diglucoside) and m/z 187.1→m/z 131.1 ( psoralen and isopsoralen ) were monitored in multiple reaction monitoring mode ( MRM) , determined by LC-MS/MS, and comparing with the results of HPLC .Result:Their average recoveries were 99.08%, 98.95%and 98.56%, with RSDs of 1.33%, 1.43%and 1.27%. Conclusion:The determination of effective components in Qing'e pill by LC-MS/MS, comparing with HPLC is simple , sensitive and accurate .