摘要
目的:建立高效液相色谱法测定黄连、黄芩药对提取物中11个成分(药根碱、表小檗碱、黄连碱、巴马汀、小檗碱、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素A)的含量。方法:采用Phenomoil 5μC18BDS(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-水(37∶63,内含磷酸二氢钾0.3400 g,十二烷基硫酸钠0.1700 g,磷酸调pH约为4),流速1.0 mL·min-1,检测波长349 nm,柱温30℃,对药对中黄连进行测定;采用Agilent ZORBAX SB-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.3%磷酸三乙胺(B)水溶液为流动相,梯度洗脱,流速1.0 mL·min-1,检测波长为275 nm,柱温30℃,对药对中黄芩进行测定。结果:药根碱、表小檗碱、黄连碱、巴马汀、小檗碱、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、白杨素、千层纸素A进样量分别在0.015~0.15μg(r=0.9997)、0.033~0.33μg(r=0.9993)、0.17~1.7μg(r=0.9991)、0.079~0.79μg(r=0.9991)、0.31~3.1μg(r=0.9991)、0.42~4.2μg(r=0.9992)、0.078~0.78μg(r=0.9995)、0.053~0.53μg(r=0.9993)、0.016~0.16μg(r=0.9993)、1.2×10-3~0.012μg(r=0.9991)、0.010~0.10μg(r=0.9994)范围内呈良好线性关系;平均回收率(n=5)分别为100.1%、97.7%、97.6%、102.2%、99.4%、99.3%、99.9%、99.8%、101.1%、101.1%、100.3%,RSD分别为2.1%、1.1%、1.2%、0.9%、1.2%、1.8%、1.8%、2.2%、2.0%、1.9%、2.3%。结论:该方法为黄芩、黄连药对提取物的质量综合评价提供了科学依据。
Objective :To establish an HPLC method for determination of eleven constituents (jatrorrhizine, epiber- berine, coptisine, palmatine, berberine, baicalin, wogonoside, baiealein, wogonin, chrysin, oroxylin- A) in combination extracts of the rhizome of Coptis chinensis Franch. and the root of Scutellaria baicalensis Georgi. Meth- ods:The Phenomoil 5μ C18 BDS column (250 mm ×4. 6 mm, 5 μm) with a column temperature of 30 ℃ was used ;the mobile phase consisted of aeetonitrile - water ( 37 : 63, containing 0. 3400 g potassium phosphate and 0. 1700 g SDS, adjusted pH to 4) with flow rate of 1.0 mL. min-1 , and the detection wavelength was set at 349 nm for determination of above - mentioned alkaloids in the rhizome of C. chinensis. And the Agilent ZORBAX SB -C18 column(250 mm ×4.6 mm, 5 μm) with a column temperature of 30 ℃ was used;the mobile phase was acetonitrile(A) -0. 3% phosphoric acid -triethylamine (B) at gradient elution program and with a flow rate of 1.0 mL.mun -1, and the detection wavelength was set at 275 nm for determination of above - mentioned flavonoids in the root of S. baicalensis. Results: The content of eleven components in combination extracts of the rhizome of C. chinensis and the root of S. baicalensis was stable. The developed method had a good linearity in the ranges of 0. 015 -0. 15 μg(r =0. 9997) for jatrorrhizine, 0. 033 -0. 33 μg(r =0. 9993) for epiberberine, 0. 17 - 1.7 μg (r = 0. 9991 ) for coptisine, 0. 079 - 0. 79 μg(r = 0. 9991 ) μg for palmatine, 0.31 - 3.1μg( r = 0. 9991 ) for ber-berine, 0. 42 -4.2 μg(r =0. 9992) for baicalin, 0. 078 -0.78 μg(r =0. 9995) for wogonoside, 0. 053 -0. 53 μg (r =0. 9993) for baicalein, 0. 016 -0. 16 μg(r =0. 9993) for wogonin, 1.2 x 10-3 -0. 012 μg(r =0. 9991 ) for ehrysin, 0. 010 -0. 10 μg(r =0. 9994) for oroxylin -A. The average reeoveries(n =5) were 100. 1%, 97.7%, 97.6%, 102.2%, 99.4%, 99.3%, 99.9%, 99.8%, 101.1%, 101.1%, 100.3% with RSDs of 2. 1%, 1.1%, 1.2%,0.9%, 1.2%, 1.8%, 1.8%, 2.2%, 2. 0%, 1.9%, 2. 3%, respectively. Conclusion: The developed method provides a scientific basis for quality assessment of combination extracts of the rhizome of C. chinensis and the root of S. baicalensis.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第1期57-62,共6页
Chinese Journal of Pharmaceutical Analysis
基金
辽宁省教育厅课题-中药材品质评价体系研究(编号:2008S145)
关键词
黄连
黄芩
药根碱
表小檗碱
黄连碱
巴马汀
小檗碱
黄芩苷
汉黄芩苷
黄芩素
汉黄芩素
白杨素
千层纸素A
高
效液相色谱
含量测定
质量评价
药对提取物
Coptis chinensis Franch.
Scutellaria baicalensis Georgi
jatrorrhizine
epiberberine
coptisine
palma-tine
berberine
baicalin
wogonoside
baicalein
wogonin
chrysin
oroxylin - A
HPLC
assay
quality evaluation
combination extracts