中国中医药信息杂志
中國中醫藥信息雜誌
중국중의약신식잡지
CHINESE JOURNAL OF INFORMATION ON TRADITIONAL CHINESE MEDICINE
2014年
6期
89-94
,共6页
王源%李梦怡%马长华%黄建梅%李莉%马恺悦%冯孟鑫
王源%李夢怡%馬長華%黃建梅%李莉%馬愷悅%馮孟鑫
왕원%리몽이%마장화%황건매%리리%마개열%풍맹흠
复方血栓通%三七皂苷R1%人参皂苷Rg1%人参皂苷Rb1%液相色谱-质谱/质谱
複方血栓通%三七皂苷R1%人參皂苷Rg1%人參皂苷Rb1%液相色譜-質譜/質譜
복방혈전통%삼칠조감R1%인삼조감Rg1%인삼조감Rb1%액상색보-질보/질보
Fufang Xueshuantong Capsule%notoginsenoside R1%ginsenoside Rg1%ginsenoside Rb1%LC-MS/MS
目的:建立复方血栓通胶囊中8种有效成分(三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rd、丹参酮Ⅰ、哈巴俄苷、黄芪甲苷)在大鼠血浆中的液相色谱-质谱/质谱定量测定方法。方法色谱柱:Thermo Hypersil GOLD(2.1 mm×100 mm,5μm);柱温:30℃;流动相:A为1%甲酸,B为乙腈;梯度洗脱:0~10 min 25%~55%B,10~20 min 55%~70%B;流速:0.2 mL/min;进样量:10μL。离子源:ESI源,正离子模式,SRM扫描。结果以盐酸巴马汀为内标,三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd、哈巴俄苷、黄芪甲苷、丹参酮Ⅰ的检测范围分别为1.00~800 ng/mL、0.950~760 ng/mL、1.44~1440 ng/mL、1.33~1330 ng/mL、9.90~990 ng/mL、1.01~1010 ng/mL、1.16~928 ng/mL、10.0~800 ng/mL。准确度分别在85%~115%之间,绝对回收率达到50%~70%,日内精密度与日间精密度RSD≤15%。结论该方法快速、灵敏、重复性好,可用于复方血栓通胶囊8种有效成分在大鼠体内的相关药代动力学研究。
目的:建立複方血栓通膠囊中8種有效成分(三七皂苷R1、人參皂苷Rg1、人參皂苷Rb1、人參皂苷Re、人參皂苷Rd、丹參酮Ⅰ、哈巴俄苷、黃芪甲苷)在大鼠血漿中的液相色譜-質譜/質譜定量測定方法。方法色譜柱:Thermo Hypersil GOLD(2.1 mm×100 mm,5μm);柱溫:30℃;流動相:A為1%甲痠,B為乙腈;梯度洗脫:0~10 min 25%~55%B,10~20 min 55%~70%B;流速:0.2 mL/min;進樣量:10μL。離子源:ESI源,正離子模式,SRM掃描。結果以鹽痠巴馬汀為內標,三七皂苷R1、人參皂苷Rg1、人參皂苷Re、人參皂苷Rb1、人參皂苷Rd、哈巴俄苷、黃芪甲苷、丹參酮Ⅰ的檢測範圍分彆為1.00~800 ng/mL、0.950~760 ng/mL、1.44~1440 ng/mL、1.33~1330 ng/mL、9.90~990 ng/mL、1.01~1010 ng/mL、1.16~928 ng/mL、10.0~800 ng/mL。準確度分彆在85%~115%之間,絕對迴收率達到50%~70%,日內精密度與日間精密度RSD≤15%。結論該方法快速、靈敏、重複性好,可用于複方血栓通膠囊8種有效成分在大鼠體內的相關藥代動力學研究。
목적:건립복방혈전통효낭중8충유효성분(삼칠조감R1、인삼조감Rg1、인삼조감Rb1、인삼조감Re、인삼조감Rd、단삼동Ⅰ、합파아감、황기갑감)재대서혈장중적액상색보-질보/질보정량측정방법。방법색보주:Thermo Hypersil GOLD(2.1 mm×100 mm,5μm);주온:30℃;류동상:A위1%갑산,B위을정;제도세탈:0~10 min 25%~55%B,10~20 min 55%~70%B;류속:0.2 mL/min;진양량:10μL。리자원:ESI원,정리자모식,SRM소묘。결과이염산파마정위내표,삼칠조감R1、인삼조감Rg1、인삼조감Re、인삼조감Rb1、인삼조감Rd、합파아감、황기갑감、단삼동Ⅰ적검측범위분별위1.00~800 ng/mL、0.950~760 ng/mL、1.44~1440 ng/mL、1.33~1330 ng/mL、9.90~990 ng/mL、1.01~1010 ng/mL、1.16~928 ng/mL、10.0~800 ng/mL。준학도분별재85%~115%지간,절대회수솔체도50%~70%,일내정밀도여일간정밀도RSD≤15%。결론해방법쾌속、령민、중복성호,가용우복방혈전통효낭8충유효성분재대서체내적상관약대동역학연구。
Objective To establish a sensitive and specific LC-MS/MS method for measurement of notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, tanshinone Ⅰ, astragaloside Ⅳ and harpagosidein of Fufang Xueshuantong Capsule in rat plasma. Methods The HPLC separation was performed on Thermo Hypersil GOLD column (2.1 mm× 100mm, 5 μm) at 30 ℃, injecting 10 μL and using acetonitrile-water (0.1% formic acid) as the mobile phrase (B was acetonitrile, A was 0.1%formic acid;0-10 min, 25%-55%B;10-20 min, 55%-70%B) with the flow rate of 0.2 mL/min. Detection was performed on a tandem quadrapole mass spectrometer using positive electrospray ionization, SRM scan mode. Results The eight compounds showed good linearity in wide ranges (notoginsenoside R1 1.00-800 ng/mL, ginsenoside Rg1 0.950-760 ng/mL, ginsenoside Re 1.44-1440 ng/mL, ginsenoside Rb1 1.33-1330 ng/mL, ginsenoside Rd 9.90-990 ng/mL, harpagosidein 1.01-1010 ng/mL, astragaloside Ⅳ 1.16-928 ng/mL, tanshinone Ⅰ 10.0-800 ng/mL). In addition, the accuracy and recovery were around 85%-115%and 50%-70%. The RSD of intra and inter day precision were lower than 15%. Conclusion The method is specific, rapid and sensitive. Therefore, it can be applied to pharmacokinetic study of eight effective compounds in Fufang Xueshuantong Capsule.