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作 者:殷燕 刘玉宁 王佩 刘艳萍 袁志兵 谢和兵 YIN Yan;LIU Yuning;WANG Pei;LIU Yanping;YUAN Zhibing;XIE Hebing(School of Pharmacy,Anhui University of Chinese Medicine,Hefei Anhui 230012,China;Yangtze Delta Drug Advanced Research Institute,Nantong Jiangsu 226133,China;Jiangsu Shenhou Pharmaceutical Research Co.,Ltd.,Nantong Jiangsu 226133,China;Xizang Shenhou Pharmaceutical Co.,Ltd.,Shigatse Xizang 857000,China)
机构地区:[1]安徽中医药大学药学院,安徽合肥230012 [2]南通市海门长三角药物高等研究院,江苏南通226133 [3]江苏神猴医药研究有限公司,江苏南通226133 [4]西藏神猴药业有限责任公司,西藏日喀则857000
出 处:《中医药导报》2024年第11期60-63,共4页Guiding Journal of Traditional Chinese Medicine and Pharmacy
基 金:国家自然科学基金项目(81470247);西藏自治区科技厅区域科技协同创新专项(QYXTZX-RKZ2022-07)。
摘 要:目的:建立高效液相色谱(HPLC)法测定藏药四味石榴丸中主要指标成分没食子酸、鞣花酸、桂皮醛、胡椒碱含量的方法。方法:采用Ultimate XB-C18液相色谱柱(250.0 mm×4.6 mm,5.0μm),柱温30℃,0.1%磷酸水溶液(A)-60.0%乙腈甲醇溶液(B)梯度洗脱(0~50 min,5.0%B→90.0%B),流速1.0 mL/min,检测波长270 nm,进样量10μL。结果:没食子酸、鞣花酸、桂皮醛和胡椒碱线性范围分别为1.91~38.10μg/mL(r=1.0000)、1.69~33.76μg/mL(r=0.9996)、1.05~21.08μg/mL(r=1.0000)、5.24~104.76μg/mL(r=1.0000);定量限分别为7.62、6.75、2.09、10.48 ng/mL;检测限分别为2.67、2.36、0.73、3.67 ng/mL;精密度(RSD值分别为0.37%、0.24%、0.16%、0.17%)、重复性(RSD值分别为1.05%、2.21%、2.84%、1.16%)、稳定性(RSD值分别为1.76%、1.28%、0.67%、0.67%)良好;平均加样回收率分别为102.7%(RSD=1.72%)、103.6%(RSD=4.11%)、103.5%(RSD=2.03%)、107.1%(RSD=0.88%)。结论:经方法学验证,该方法可用于藏药四味石榴丸中没食子酸、鞣花酸、桂皮醛、胡椒碱的含量测定。Objective:To establish a HPLC method for the determination of gallic acid,ellagic acid,cinnamic aldehyde and piperine in Zang medicine Siwei pomegranate pills.Methods:The HPLC column was Ultimate XB-C18(250.0 mm×4.6 mm,5.0μm),and the column temperature was 30℃.Gradient elution(0~50 min,5%B→90%B)was performed with 0.1%phosphoric acid water solution(A)-60%acetonitrile methanol solution(B),and the total flow rate was 1.0 mL/min.The detection wavelength was 270 nm,and the sample size was 10μL.Results:The linear ranges of gallic acid,ellagic acid,cinnamic aldehyde and piperine were 1.91~38.10μg/mL(r=1.0000),1.69~33.76μg/mL(r=0.9996),1.05~21.08μg/mL(r=1.0000)and 5.24~104.76μg/mL(r=1.0000),respectively.The limits of quantification were 7.62,6.75,2.09 and 10.48 ng/mL,respectively.The detection limits were 2.67,2.36,0.73 and 3.67 ng/mL,respectively.The precision(RSD=0.37%,0.24%,0.16%,0.17%),repeatability(RSD=1.05%,2.21%,2.84%,1.16%)and stability(RSD=1.76%,1.28%,0.67%,0.67%)were good.The average recoveries were 102.7%(RSD=1.72%),103.6%(RSD=4.11%),103.5%(RSD=2.03%)and 107.1%(RSD=0.88%),respectively.Conclusion:The method is proved to be suitable for the determination of gallic acid,ellagic acid,cinnamic aldehyde and piperine in Zang medicine Siwei pomegranate pills.
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