目的:建立超高效液相色谱法同时测定三黄睛视明丸中香蒲新苷、毛蕊异黄酮苷、异鼠李素-3-O-新橙皮苷、芒柄花苷、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1和人参皂苷Rd 9个成分的含量。方法:采用Waters Acquity UPLC® BEH C18色谱柱(2.1 mm×100 mm,1.7 μm),柱温30℃,流动相为水(A)-乙腈(B),梯度洗脱,流速0.3 mL·min-1,检测波长203 nm。结果:香蒲新苷、毛蕊异黄酮苷、异鼠李素-3-O-新橙皮苷、芒柄花苷、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd的线性范围分别为1.92~36.94 ng(r=0.999 8)、1.90~36.63 ng(r=0.999 9)、1.88~36.20 ng(r=0.999 6)、0.99~19.09 ng(r=0.999 2)、40.04~770.05 ng(r=0.999 8)、107.78~2 072.68 ng(r=0.999 8)、31.74~610.34 ng(r=0.999 1)、81.33~1 564.08 ng(r=0.999 9)、19.711~379.06 ng(r=0.999 9);平均回收率(n=6)均在91%~105%之间,RSD均小于3.0%。测定的3批样品中上述9个成分含量范围分别为0.261~0.294、0.196~0.209、0.189~0.193、0.101~0.111、2.728~2.773、12.051~12.196、3.235~3.313、8.317~8.464、2.131~2.229 mg·g-1。结论:所建立的多成分含量测定方法可用于三黄睛视明丸质量控制。
Objective:To establish a UPLC method for the simultaneous determination of nine constituents in Sanhuang Jingshiming pills, including typhaneoside, calycosin-7-O-β-D-glucopyranoside, isorhamnetin-3-O-neohesperidoside, ononin, notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, and ginsenoside Rd. Methods:The UPLC analysis was carried out by a 30 thermostatic Waters Acquity UPLC® BEH C18 column (2.1 mm×100 mm, 1.7 μm) with a mobile phase composed of acetonitrile-water for gradient elution at 0.3 mL·min-1. The detection wavelength was 203 nm. Results:The calibration curves of typhaneoside, calycosin-7-O-β-D-glucopyranoside, isorhamnetin-3-O-neohesperidoside, ononin, notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, and ginsenoside Rd were in good linearity over the ranges of 1.92-36.94 ng(r=0.999 8), 1.90-36.63 ng(r=0.999 9), 1.88-36.20 ng(r=0.999 6), 0.99-19.09 ng(r=0.999 2), 40.04-770.05 ng(r=0.999 8), 107.78-2 072.68 ng(r=0.999 8), 31.74-610.34 ng(r=0.999 1), 81.33-1 564.08 ng(r=0.999 9), 19.71-379.06 ng(r=0.999 9), respectively. The average recoveries(n=6) varied from 91%-105% with RSDs no more than 3.0%. The content ranges of the above mentioned 9 components in 3 batches of samples were 0.261-0.294, 0.196-0.209, 0.189-0.193, 0.101-0.111, 2.728-2.773, 12.051-12.196, 3.235-3.313, 8.317-8.464, and 2.131-2.229 mg·g-1, respectively. Conclusion:This method can be used for quality control of Sanhuang Jingshiming pills.