摘要
目的 建立同时测定乙肝解毒胶囊中没食子酸、香草酸、胡黄连苷Ⅱ、落新妇苷、黄杞苷、胡黄连苷Ⅰ、黄芩苷、盐酸小檗碱、汉黄芩苷、大黄酚、大黄素和汉黄芩素12种成分的含量测定方法。方法 以十八烷基键合硅胶为填充剂(Waters Atlantic T3 C18色谱柱),乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱(0~10 min,4%→13%A;10~20 min,13%→15%A;20~25 min,15%→19%A;25~35 min,19%A;35~36 min,19%→23%A;36~45 min,23%→27%A;45~56 min,27%→43%A;56~65 min,43%→65%A),柱温40 ℃,流速1 mL·min-1,波长切换,0~22 min,270 nm;22~44 min,290 nm;44~65 min,270 nm。结果 12种成分可以实现完全分离,并与其他成分均能达到良好的分离;没食子酸、香草酸、胡黄连苷Ⅱ、落新妇苷、黄杞苷、胡黄连苷Ⅰ、黄芩苷、盐酸小檗碱、汉黄芩苷、大黄素、大黄酚和汉黄芩素的进样量分别在0.012 19～0.243 8 μg,0.036 70～0.734 0 μg,0.033 77～0.675 4 μg,0.057 38～1.147 6 μg,0.006 580～0.131 6 μg,0.015 38～0.307 6 μg,0.067 11～1.342 2 μg,0.028 04～0.560 8 μg,0.041 48～0.829 6 μg,0.006 310～0.126 2 μg,0.013 64～0.272 8 μg和0.014 22～0.284 4 μg内,与色谱峰峰面积呈良好线性响应;平均回收率(n=6)分别为98.7%,98.9%,99.4%,99.2%,98.9%,99.1%,98.9%,99.6%,99.3%,98.9%,98.6%和99.0%;RSD分别为1.02%,0.46%,0.64%,0.86%,1.1%,1.3%,0.60%,0.92%,0.61%,1.5%,0.93%和0.98%。结论 该方法多种成分同时测定,操作简便,准确、重复性好,可用于乙肝解毒胶囊的质量控制。
Abstract
OBJECTIVE To develop a method for determining 12 constituents in Yigan Jiedu Capsules by HPLC. METHODS The quantitative analysis was carried out on a Waters Atlantic T3 C18column maintained at 40 ℃, using mobile phase consisting of acetonitrile(A)and 0.1% phosphoric acid solution(B)by a gradient elution program(0-10 min, 4%→13%A; 10-20 min, 13%→15%A; 20-25 min, 15%→19%A; 25-35 min, 19%A; 35-36 min, 19%→23%A; 36-45 min, 23%→27%A; 45-56 min, 27%→43%A; 56-65 min, 43%→65%A) at a flow rate of 1 mL·min-1. The detection wavelength was set at 270 nm in the first 22 min, and then changed to 290 nm between 22 and 44 min, and last changed to 270 nm. RESULTS The linear ranges of gallic acid, vanillic acid, picroside Ⅱ, astilbin, engeletin, picrosideⅠ, baicalin, berberine hydrochloride, wogonoside, emodin, chrysophanol and wogonin fell with in the range of 0.012 19-0.243 8 μg, 0.036 70-0.734 0 μg, 0.033 77-0.675 4 μg, 0.057 38-1.147 6 μg, 0.006 580-0.131 6 μg, 0.015 38-0.307 6 μg, 0.067 11-1.342 2 μg, 0.028 04-0.560 8 μg, 0.041 48-0.829 6 μg, 0.006 310-0.126 2 μg, 0.013 64-0.272 8 μg and 0.014 22-0.284 4 μg. The recoveries were 98.7%, 98.9%, 99.4%, 99.2%, 98.9%, 99.1%, 98.9%, 99.6%, 99.3%, 98.9%, 98.6% and 99.0%, respectively. The relative standard deviations were 1.02%, 0.46%, 0.64%, 0.86%, 1.1%, 1.3%, 0.60%, 0.92%, 0.61%, 1.5%, 0.93%and 0.98%, respectively(n=6). CONCLUSION This method is simple, accurate, reproducible and convenient for the quality control over Yigan Jiedu Capsules.
关键词
高效液相色谱法 /
乙肝解毒胶囊 /
土茯苓 /
胡黄连 /
黄柏 /
黄芩 /
大黄 /
多种成分同时测定
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Key words
HPLC /
Yigan Jiedu Capsules /
Smilacis Glabrae Rhizoma /
Picrorhizae Rhizoma /
Phellodendri Chinensis Cortex /
Scutellariae Radix /
Rhei Rsdix et Rhizoma /
simultaneou differmination
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林林, 刘广桢, 于凤蕊, 林永强.
高效液相色谱法同时测定乙肝解毒胶囊中12种成分的含量[J]. 中国药学杂志, 2020, 55(7): 557-561 https://doi.org/10.11669/cpj.2020.07.012
LIN Lin, LIU Guang-zhen, YU Feng-rui, LIN Yong-qiang.
Simultaneous Determination of Twelve Constituents in Yigan Jiedu Capsules by HPLC[J]. Chinese Pharmaceutical Journal, 2020, 55(7): 557-561 https://doi.org/10.11669/cpj.2020.07.012
中图分类号：
R917
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参考文献
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脚注
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基金
山东省自然科学基金项目资助(ZR2013HM074)
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