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作 者:王健芬 孟纯燕 尹兴章 张枝雪 Wang Jianfen;Meng Chunyan;Yin Xingzhang;Zhang Zhixue(Baoshan Inspection and Testing Center for Food and Drug,Baoshan 678000,China;Baoshan College of Traditional Chinese Medicine,Baoshan 678000,China)
机构地区:[1]保山市食品药品检验检测中心,云南保山678000 [2]保山中医药高等专科学校,云南保山678000
出 处:《云南化工》2024年第9期77-81,共5页Yunnan Chemical Technology
基 金:保山中医药高等专科学校2024年校级科技计划项目,项目编号:2023k005;云南省教育厅科学研究基金项目,项目编号:2022J15730。
摘 要:(目的)建立测定龙胆泻肝片中龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素等含量的高效液相色谱的方法。(方法)色谱柱为Agilent ZORBAX SB-Aq C 8(4.6 mm×250 mm,5μm);以乙腈溶液为流动相A,以0.1%磷酸的水溶液为流动相B,进行梯度洗脱;龙胆苦苷、栀子苷检测波长为254 nm,黄芩苷、汉黄芩苷、黄芩素、汉黄芩素检测波长为280nm;流速为1mL/min;柱温为30℃。(结果)龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素的线性范围分别为:26.64~159.84 mg/mL,r=0.9997;13.15~78.91 mg/mL,r=0.9997;40.98~245.88 mg/mL,r=0.9998;8.53~51.17 mg/mL,r=0.9999;3.95~23.69 mg/mL,r=0.9998;2.18~13.07 mg/mL,r=0.9999。平均回收率分别为99.2%、100.1%、99.2%、98.6%、99.2%和100.9%,RSD分别为1.64%、0.45%、0.89%、0.65%、1.29%和1.78%。测定24批样品,结果表明,龙胆泻肝片中每片含龙胆苦苷、栀子苷、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素的质量分别在0.872~3.933 mg、0.676~1.908 mg、1.951~6.840 mg、0.729~3.289 mg、0.527~3.195 mg和0.070~0.485 mg。(结论)该方法操作简便、重复性好、结果准确,可作为龙胆泻肝片的控制方法。(Objective)Establish a method for determining the contents of gentiopicroside,geniposide,baicalin,baicalein,wogonoside and wogonin in Longdan Xiegan tablets by HPLC.(Methods)Agilent ZORBAX SB-Aq C 8(4.6 mm×250 mm,5μm)chromatographic column;Perform gradient elution using acetonitrile solution as mobile phase A and aqueous solution containing 0.1%phosphoric acid as mobile phase B;Detection wavelength for gentiopicroside and geniposide:254 nm;baicalin,baicalein,wogonoside and wogonin:280 nm;The flow rate is 1 mL/min;The column temperature is 30℃.(Results)The linear ranges of gentiopicroside,geniposide,baicalin,baicalein,wogonoside and wogonin are 426.64~159.84 mg/mL,r=0.9997;13.15~78.91 mg/mL,r=0.9997;40.98~245.88 mg/mL,r=0.9998;8.53~51.17 mg/mL,r=0.9999;3.95~23.69 mg/mL,r=0.9998;2.18~13.07 mg/mL,r=0.9999.The average recovery rates are 99.2%,100.1%,99.2%,98.6%,99.2%,and 100.9%,The RSD values are 1.64%,0.45%,0.89%,0.65%,1.29%,and 1.78%.24 batches of samples were determined,and the results showed that each tablet of Longdan Xiegan tablets contained amounts of gentiopicroside,geniposide,baicalin,baicalein,wogonoside and wogonin ranging from 0.872 to 3.933 mg,0.676 to 1.908 mg,1.951 to 6.840 mg,0.729 to 3.289 mg,0.527 to 3.195 mg,and 0.070 to 0.485 mg.(Conclusion)This method is easy to operate,has good repeatability,and accurate results,and can be used as a control method for Longdan Xiegan tablets.
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