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刊物信息

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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枳壳HPLC特征图谱及6个黄酮苷类成分含量测定

Study on characteristic chromatogram and quantitation method of six components in Aurantii Fructus

分类号:R917
出版年·卷·期(页码):2020,40 (6):1090-1096
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 采用高效液相色谱法建立枳壳的特征图谱,并同时测定6个黄酮苷类成分的含量。方法: 以新北美圣草苷、芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷和枳属苷为指标性成分,采用Kinetex? 2.6 μ C18 100(100 mm×4.6 mm,2.6 μm)色谱柱,以乙腈为流动相B,0.1%甲酸为流动相A,梯度洗脱(0~10 min,15% B→15% B;10~15 min,15% B→20% B;15~20 min,20% B→25% B;20~30 min,25% B→40% B),流速1.0 mL·min-1,检测波长为283 nm,柱温30℃。结果: 建立枳壳特征图谱,30 min内枳壳的主要色谱峰能够达到完全分离,同时标定6个黄酮苷类成分,对12批饮片中的6个成分进行含量测定。新北美圣草苷、芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷和枳属苷的质量浓度分别在1.77~70.8 μg·mL-1r=0.999 8,n=5)、11.3~452.0 μg·mL-1(r=1.000 0,n=5)、34.0~1 360 μg·mL-1r=0.999 9,n=5)、13.6~544 μg·mL-1r=1.000,n=5)、27.6~1 104 μg·mL-1r=0.999 6,n=5)、14.9~596 μg·mL-1r=1.000,n=5)范围内线性关系良好,方法的平均回收率(n=6)分别为96.9%(RSD=1.8%)、104.6%(RSD=1.7%)、97.4%(RSD=1.11%)、107.4%(RSD=1.1%)、93.2%(RSD=1.1%)、107.8%(RSD=1.5%);12批枳壳中上述6个成分含量分别为0.11%~0.45%、0.17%~0.59%、4.85%~9.09%、0.37%~0.74%、3.24%~6.17%、0.05%~0.56%。结论: 该方法操作简单,重复性好,并能同时测定6个黄酮苷类成分含量,可为枳壳的质量标准研究提供更加全面的依据。

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

Objective: To establish an HPLC characteristic chromatogram and quantitative method for six components in Aurantii Fructus.Method: With neoeriocitrin,narirutin,naringin,hesperidin,neohesperidin and poncirin as reference substances,HPLC analysis was performed on a Kinetex? 2.6 μ C18 100 A column(100 mm×4.6 mm,2.6 μm)with the gradient elution of acetonitrile(B)-0.1% formic acid solution(A)(0-10 min,15%B→15%B;10-15 min,15%B→20%B;15-20 min,20%B→25%B;20-30 min,25%B→40%B). The flow rate was 1.0 mL·min-1,the detection wavelength was 283 nm and the column temperature was 30℃. Results: HPLC characteristic chromatogram of Aurantii Fructus was established and six characteristic peaks were marked.Six characteristic peaks were simultaneously determined by HPLC within 30 min.The linear ranges of neoeriocitrin,narirutin,naringin,hesperidin,neohesperidin and poncirin were 1.77-70.8 μg·mL-1(r=0.999 8,n=5),11.3-452.0 μg·mL-1(r=1.000,n=5),34.0-1 360 μg·mL-1(r=0.999 9,n=5),13.6-544 μg·mL-1(r=1.000,n=5),27.6-1 104 μg·mL-1(r=0.999 6,n=5)and 14.9-596 μg·mL-1(r=1.000,n=5),respectively.The average recovery rate(n=6)were 96.9%(RSD=1.8%),104.6%(RSD=1.7%),97.4%(RSD=1.1%),107.4%(RSD=1.1%),93.2%(RSD=1.1%)and 107.8%(RSD=1.5%),respectively.The contents of the six components in 12 batches of Aurantii Fructus were 0.11%-0.45%,0.17%-0.59%,4.85%-9.09%,0.37%-0.74%,3.24%-6.17% and 0.05%-0.56%,respectively.Conclusion: The proposed specific HPLC characteristic chromatogram and quantitation method of six components for Aurantii Fructus are simple and repeatable,which offer reference for quality control of the drug.

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