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UHPLC - MS / MS 法同时测定甘地胶囊中 7 个成分的含量
  • ISSN号:0254-1793
  • 期刊名称:《药物分析杂志》
  • 时间:0
  • 分类:R917[医药卫生—药物分析学;医药卫生—药学]
  • 作者机构:[1]第二军医大学药学院,上海200433, [2]上海交通大学医学院附属新华医院,上海200092
  • 相关基金:上海市科委项目(N0.11DZ1972500,No.12DZ1930404);国家自然科学基金(No.81202598);上海市教委创新基金(No.12ZZ117)
中文摘要:

目的:建立甘地胶囊中咖啡酸、阿魏酸、芦丁、野黄芩苷、黄芩苷、黄芪甲苷、汉黄芩素7个成分的UHPLC—MS/MS测定方法。方法:采用ZORBAXSB—C18(2.1mm×50mm,1.8μm)色谱柱,以乙腈(A)一水(B)为流动相,梯度洗脱(0—4min,5%A-20%A;4~4.5min,20%A→40%A;4.5—8min,40%A→43%A;8—8.5min,43%A→90%A;8.5~9min,90%A→5%A),流速0.4mL·min^-1,柱温35℃;采用电喷雾离子源(ESI),多反应离子监测(MRM),结合正负离子扫描切换,其中咖啡酸、阿魏酸、野黄芩苷采用负离子模式检测,芦丁、黄芩苷、黄芪甲苷、汉黄芩素采用正离子模式检测。结果:咖啡酸、阿魏酸、芦丁、野黄芩苷、黄芩苷、黄芪甲苷、汉黄芩素的定量下限分别为0.22、0.35、0.39、0.48、0.31、1.31、0.11ng·mL^-1,检测下限分别为0.066、0.11、0.12、0.14、0.092、0.39、0.033ng·mL^-1;在相应的线性范围内相关系数〉0.99;日内和日间精密度(RSD)均小于5%,平均回收率均为80%~120%。结论:经方法学验证,本方法简单、快速、灵敏、准确,可用于甘地胶囊中咖啡酸、阿魏酸、芦丁、野黄芩苷、黄芩苷、黄芪甲苷、汉黄芩素7个成分的含量测定。通过对18个批次甘地胶囊进行测定,结果显示各个批次含量有较明显差别,同时随着时间推移,含量略有下降趋势,尤其以芦丁和黄芩苷的变化趋势较明显,可为该药的质量控制提供依据。

英文摘要:

Objective: To establish a UHPLC - MS/MS method for simultaneous determination of caffeic acid,ferulic acid, rutin, scutellarin, baicalin, astragaloside IV, wogonin in Gandi capsules. Methods: The chromatographic separation was on ZORBAX SB -C 18 column (2. 1 mm× 50 mm, 1.8 μm) with a mobile phase consisting of acetonitrile (A) -water (B) at a flow rate of 0.4 mL· min^-1(0 -4 min,5%A→20%A;4 -4. 5 min,20% A→40% A;4. 5 -8 min, 40% A→3 % A ; 8 - 8. 5 min,43 % A→90% A ; 8. 5 - 9 min,90% A→5% A), and the column temperature was 35 ℃, using electrospray ionization source (ESI), and muhiple reaction monitoring (MRM), combined with positive and negative scanning switch. Caffeic acid, ferulic acid, and scutellarin were detected using negative ion mode,while rutin, baicalin,as- tragaloside IV,and wogonin were detected using positive ion mode. Results: The quantification limits of caffeic acid ,feru- lie acid, rutin, seutellarin, baicalin, astragaloside IV, and wogonin were 0. 22,0. 35, 0. 39,0. 48,0. 31,1.31,0. 11 ng · mL^-1 ,and the detection limits were 0. 066,0. 11,0. 12,0. 14,0. 092,0. 39,0. 033 ng· mL^-1 ,respectively. Within the linear range,the correlation coefficient was 〉0. 99. Intraday and inter- day precisions (RSDs) were less than 5%. The aver- age recoveries of the seven components were in the range of 80% - 120%. Conclusion: By method validation ,this method is proved to be simple,rapid, sensitive and accurate. It can be used to determine eaffeic acid ,ferulic acid, rutin, scutel-larin ,baicalin, astragaloside IV, and wogonin in Gandi capsules. The determination results of 18 batches of Gandi capsules showed that the content of each batch had significant difference, and the content had a slight decreasing trend over time, especially for rutin and baicalin. These results were helpful for the quality control of drug.

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期刊信息
  • 《药物分析杂志》
  • 中国科技核心期刊
  • 主管单位:中国科协
  • 主办单位:中国药学会
  • 主编:金少鸿
  • 地址:北京天坛西里2号
  • 邮编:100050
  • 邮箱:ywfx@nifdc.org.cn
  • 电话:010-67058427
  • 国际标准刊号:ISSN:0254-1793
  • 国内统一刊号:ISSN:11-2224/R
  • 邮发代号:2-237
  • 获奖情况:
  • 四通杯全优期刊奖,92、97年获科协优秀期刊三等奖,96年影响因子全年第一
  • 国内外数据库收录:
  • 美国国际药学文摘,美国化学文摘(网络版),日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:32603