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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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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

分类号:R917
出版年·卷·期(页码):2019,39 (11):1992-1997
DOI: 10.16155/j.0254-1793.2017.01.01
-----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,5 μm);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10 μL。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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------

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