中国药房2017，Vol.28Issue(21)：2959-2963,5.DOI:10.6039/j.issn.1001-0408.2017.21.22
UPLC-MS/MS法同时测定复方血栓通胶囊中9种成分的含量
Simultaneous Determination of 9 Components in Compound Xueshuantong Capsules by UPLC-MS/MS
摘要
Abstract
OBJECTIVE:To establish a method for simultaneous determination of tanshinol,caffeic acid,rosmarinic,salviano-lic acid B,salvianolic acid A,tanshinoneⅠ,cryptotanshinone,tanshinone ⅡA and ursolic acid in Compound xueshuantong cap-sules. METHODS:UPLC-MS/MS method was adopted. The determination was performed on ACQUITY UPLC? BEH C18 column with mobile phase consisted of acetonitrile-0.1%formic acid(gradient elution)at the flow rate of 0.2 mL/min. The column tempera-ture was 40 ℃,and the temperature of injector was 10 ℃. Analysis time was 7 min,and sample size was 5 μL. The electrospray ionization source(ESI)was used;ion source temperature was 150℃;capillary voltage was 3.5 kV;cone flow was 50 L/h;desol-vation temperature was 350 ℃;desolvation gas flow was 650 L/h;nebuliser pressure was 7 × 105 Pa;ion monitoring and multiple reaction monitoring (MRM) was performed. RESULTS:The linear ranges of tanshinol,caffeic acid,rosmarinic,salvianolic acid B,salvianolic acid A,tanshinoneⅠ,cryptotanshinone,tanshinone ⅡA and ursolic acid were 10.0-100.0 μg/mL (r=0.9998), 0.1-1.0 μg/mL(r=0.9998),4.0-40.0 μg/mL(r=0.9999),10.0-100.0 μg/mL(r=0.9999),15.0-150.0 μg/mL(r=0.9997), 8.0-80.0 μg/mL(r=0.9998),10.0-100.0 μg/mL(r=0.9997),50.0-500.0 μg/mL(r=0.9997)and 6.0-60.0 μg/mL(r=0.9998), respectively. The limits of quantitation were 40.0,9.6,38.0,88.0,130.0,39.0,4.4,3.2 and 10.0 ng/mL,separately. The limits of detection were 12.0,3.0,11.0,26.0,39.0,12.0,1.3,1.0 and 3.0 ng/mL,respectively. RSDs of precision,stability and repro-ducibility tests were all lower than 3%. The recoveries were 97.34%-103.20%(RSD=2.19%,n=6),97.22%-102.39%(RSD=2.03%,n=6),98.51%-101.70%(RSD=1.32%,n=6),97.86%-102.49%(RSD=2.09%,n=6),96.75%-103.12%(RSD=2.36%,n=6),98.43%-101.65%(RSD=1.25%,n=6), 97.59%-101.50%(RSD=1.50%,n=6), 96.45%-102.88%(RSD=2.58%,n=6),97.02%-103.11%(RSD=2.38%,n=6),separately. CONCLUSIONS:The method is simple and accurate,and can be used for simultaneous determination of 9 components in Compound xueshuantong capsules.关键词
超高效液相色谱-串联质谱法/复方血栓通胶囊/含量测定/丹参素/咖啡酸/迷迭香酸/丹酚酸B/丹酚酸A/丹参酮Ⅰ/隐丹参酮/丹参酮ⅡA/熊果酸Key words
UPLC-MS/MS/Compound xueshuantong capsules/Content determination/Tanshinol/Caffeic acid/Rosmarinic/Salvianolic acid B/Salvianolic acid A/TanshinoneⅠ/Cryptotanshinone/TanshinoneⅡA/Ursolic acid分类
医药卫生引用本文复制引用
孙志,张晓坚,胡玉荣,左莉华,周霖,姜晓芳,刘新,吕晓景,包晓悦,康建..UPLC-MS/MS法同时测定复方血栓通胶囊中9种成分的含量[J].中国药房,2017,28(21):2959-2963,5.基金项目
国家自然科学基金资助项目(No.81272563) （No.81272563）
郑州大学第一附属医院院内青年创新基金项目 （）
