HPLC法同时测定新癀片中8个成分的含量

目的: 建立HPLC法同时测定新癀片中8个成分(异嗪皮啶、迷迭香酸、三七皂苷R₁、人参皂苷Rg_l、人参皂苷Re、人参皂苷Rb₁、人参皂苷Rd、吲哚美辛)。方法: 采用Agilent ZORBAX SB-C₁₈色谱柱(4.6 mm×250 mm,5 μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~30 min,19.5%A;30~60 min,19.5%A→40%A;60~75 min,40%A→45%A;75~90 min,45%A→85%A;90~100 min,19.5%A),流速1.0 mL·min^-1,检测波长为203 nm(三七皂苷R₁、人参皂苷Rg_l、人参皂苷Re、人参皂苷Rb₁、人参皂苷Rd)、254 nm(吲哚美辛)和342 nm(异嗪皮啶、迷迭香酸),柱温30 ℃。结果: 异嗪皮啶、迷迭香酸、三七皂苷R₁、人参皂苷Rg_l、人参皂苷Re、人参皂苷Rb₁、人参皂苷Rd和吲哚美辛的线性范围分别为10.09~504.7、10.16~508.2、34.24~1 712、164.6~8 230、27.64~1 382、121.7~6 084、157.7~7 883和274.5~13 724 ng;平均加样回收率(n=3)分别为99.2%~100.3%、101.6%~103.5%、97.6%~98.1%、99.3%~100.7%、96.2 %~98.8%、101.1%~102.5%、99.8%~100.8%和101.1%~101.8%,RSD均≤3.0%。3批样品中上述8个成分的含量范围分别为0.38~0.83、0.37~0.83、2.07~2.32、12.40~17.33、1.75~2.64、6.97~11.18、10.85~12.84和19.29~20.80 mg·g^-1。结论: 该方法操作简单,重复性好,为评价和控制新癀片的质量提供了可靠的方法。

Objective: To establish a method for simultaneous determination of eight active ingredients (isofraxidin, rosmarinic acid, notoginsenoside R₁, ginsenoside Rg₁, ginsenoside Re, ginsenoside Rb₁, ginsenoside Rd, and indometaein) in Xinhuang tablets.Methods: The determination was carried out with Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5 μm).The mobile phase consisted of acetonitrile(A)-0.1% phosphoric acid solution(B) with gradient elution(0-30 min, 19.5%A;30-60 min, 19.5%A→40%A;60-75 min, 40%A→45%A;75-90 min, 45%A→85%A;90-100 min, 19.5%A) at a flow rate of 1.0 mL·min^-1.The detection wavelengths were 203 nm for notoginsenoside R₁, ginsenoside Rg₁, ginsenoside Re, ginsenoside Rb₁ and ginsenoside Rd, 254 nm for indometaein and 342 nm for isofraxidin and rosmarinic acid.The column temperature was 30 ℃.Results: The calibration curves were linear in the ranges of 10.09-504.7 ng for isofraxidin, 10.16-508.2 ng for rosmarinic acid, 34.24-1 712 ng for notoginsenoside R₁, 164.6-8 230 ng for ginsenoside Rg_l, 27.64-1 382 ng for ginsenoside Re, 121.7-6 084 ng for ginsenoside Rb₁, 157.7-7 883 ng for ginsenoside Rd, and 274.5-13 724 ng for indometaein.The average recoveries (n=3) were 99.2%-100.3%, 101.6%-103.5%, 97.6%-98.1%, 99.3%-100.7%, 96.2 %-98.8%, 101.1%-102.5%, 99.8%-100.8% and 101.1%-101.8%, respectively;RSDs were less than 3.0%.The content ranges were 0.38-0.83 mg·g^-1, 0.37-0.83 mg·g^-1, 2.07-2.32 mg·g^-1, 12.40-17.33 mg·g^-1, 1.75-2.64 mg·g^-1, 6.97-11.18 mg·g^-1, 10.85-12.84 mg·g^-1 and 19.29-20.80 mg·g^-1, respectively.Conclusion: The method is simple and repeatable, which can be applied to the quality control of Xinhuang tablets.