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?2.6μC18 100(100 mm×4.6 mm,2.6μm)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1.77~70.8μg·mL-1(r=0.999 8,n=5)、11.3~452.0μg·mL-1(r=1.000 0,n=5)、34.0~1 360μg·mL-1(r=0.999 9,n=5)、13.6~544μg·mL-1(r=1.000,n=5)、27.6~1 104μg·mL-1(r=0.999 6,n=5)、 14.9~596μg·mL-1(r=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。
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·m L-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.
作者
田芳
何小芳
谭梓君
吴孟华
张英
曹晖
马志国
TIAN Fang;HE Xiao-fang;TAN Zi-jun;WU Meng-hua;ZHANG Ying;CAO Hui;MA Zhi-guo(Research Center for PCM of Lingnan(Southern China),Jinan University,Guangzhou 510632,China;National Engineering Research Center for Modernization of Traditional Chinese Medicine Lingnan Kesourc-es Branch,Guangzhou 510632,China;College of Pharmacy,Jinan University,Guangzhou 510632,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第6期1090-1096,共7页
Chinese Journal of Pharmaceutical Analysis
基金
2020年广东省重点领域研发计划(第五批)(2020B11111110005)。
