HPLC法同时测定半夏中5个代表性成分的含量  

Simultaneous determination of five representative components in Pinelliae Rhizoma by HPLC

作　　者：杨冰月[1,2] 敬勇[1] 赖月月 陈洁[1] 彭亮[2] 李敏[1] YANG Bing-yue;JING Yong;LAI Yue-yue;CHEN Jie;PENG Liang;LI Min(Key Laboratory of Standardization of Chinese Herbal Medicine,State Key Laboratory Breeding Base of Systematic Research,Development and Utilization of Chinese Medicine Resources,College of Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Shaanxi Qinling Application Development and Engineering Center of Chinese Herbal Medicine,College of Pharmacy,Shaanxi University of Chinese Medicine,Xi’an 712046,China)

机构地区：[1]成都中医药大学中药材标准化教育部重点实验室中药资源系统研究与开发利用国家重点实验室,成都611137 [2]陕西中医药大学陕西省秦岭中草药应用开发工程技术研究中心,西安712046

出　　处：《药物分析杂志》2019年第11期1992-1997,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金资助项目(No:81173492);国家中药标准行动计划项目“川贝母、半夏等7种中药饮片标准化建设”(No:ZYBZH-Y-SC-40);四川省科技厅科技成果转化项目“半夏优质高产栽培及绿色加工技术成果转化”(No:2017CC0084);金川县、丹巴县中药材科技扶贫示范基地建设(No:2017NFP0001);四川省中医药标准化研究项目—川产道地药材半夏种茎分级标准研究(2019063);“杏林学者”学科人才科研提升计划(CXTD2018016)

摘　　要：目的:建立高效液相色谱法同时测定半夏药材中肌苷、鸟苷、腺苷、琥珀酸、盐酸麻黄碱5个代表性成分含量。方法:采用Agilent Eclipse XDB C18色谱柱(4.6 mm×250 mm,5μm);以乙腈(A)-水(B)为流动相,梯度洗脱;流速1.0 mL·min-1;检测波长265 nm;柱温30℃;进样量10μL。结果:半夏样品中5个成分的色谱峰均达到基线分离,肌苷、鸟苷、腺苷、琥珀酸、盐酸麻黄碱的线性方程分别为Y=769.1X+3.364(r=0.999 7)、Y=826.3X-7.726(r=0.999 6)、Y=841.7X-0.700 6(r=0.999 3)、Y=253.3X+1.821(r=0.999 6)、Y=362.7X+1.530(r=0.999 3);平均加样回收率分别为99.2%(RSD=1.1%)、101.4%(RSD=1.4%)、99.4%(RSD=1.0%)、99.3%(RSD=1.3%)、100.8%(RSD=0.91%);10批半夏药材中5个成分含量分别为肌苷0.21~0.33 mg·g-1、鸟苷2.02~2.18 mg·g-1、腺苷2.42~2.70 mg·g-1、琥珀酸3.24~4.43 mg·g-1、盐酸麻黄碱5.89~6.74 mg·g-1。结论:建立的半夏中5个代表性成分含量测定方法准确灵敏,稳定性和重复性好,可为半夏的质量控制提供研究方法。Objective:To establish an HPLC method for the simultaneous determination of five representative components of inosine,guanosine,adenosine,succinic acid and ephedrine hydrochloride in Pinelliae Rhizoma.Method:Samples were analyzed on an Agilent Eclipse XDB C18 column(4.6 mm×250 mm,5 μm)with the mobile phase of acetonitrile(A)and water(B)in a gradient elution.The flow rate of the mobile phase,detection wavelength,column temperature and injection volume were set at 1.0 mL·min-1,265 nm,30 ℃ and 10 μL,respectively.Results:The chromatographic peaks of the five components in the Pinelliae Rhizoma samples were all separated at baseline.The linear equations of inosine,guanosine,adenosine,succinic acid and ephedrine hydrochloride were Y=769.1X+3.364(r=0.999 7),Y=826.3X-7.726(r=0.999 6),Y=841.7X-0.700 6(r=0.999 3),Y=253.3X+1.821(r=0.999 6)and Y=362.7X+1.530(r=0.999 3),respectively;The recoveries were 99.2%(RSD=1.1%),101.4%(RSD=1.4%),99.4%(RSD=1.0%),99.3%(RSD=1.3%),and 100.8%(RSD=0.91%),respectively.The contents of the above-mentioned five components in 10 batches of Pinelliae Rhizoma were 0.21-0.33 mg·g-1,2.02-2.18 mg·g-1,2.42-2.70 mg·g-1,3.24-4.43 mg·g-1 and 5.89-6.74 mg·g-1,respectively.Conclusion:The established method for determination of five representative components in Pinelliae Rhizoma is accurate,stable and reproducible,and can provide a research method for quality control of Pinelliae Rhizoma.

关 键 词：半夏 肌苷 鸟苷 腺苷 琥珀酸 盐酸麻黄碱 高效液相色谱 含量 

分 类 号：R917[医药卫生—药物分析学]