ABSTRACT
Objective To establish an HPLC-DAD method for the simultaneous determination of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone in Yifei Qinghua Granules (YQG). Methods The chromatographic separation was achieved on an Waters Symmetry-C18 (250 mm × 4.6 mm, 5.0 μm) column with mobile phase consisted of (1.0 g potassium phosphate monobasic in 1 000 mL water, the pH value was adjusted to 3.5 with phosphate)- (acetonitrile-methanol 1:1) for gradient elution, at the flow rate of 0.8 mL/min; The column temperature was 40 ℃. Results The linear ranges of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone were 0.2-2.0 μg/mL (r = 0.999 4), 0.4-4.0 μg/mL (r = 0.999 4), 0.3-3.0 μg/mL (r = 0.999 6), 0.1-1.0 μg/mL (r = 0.999 3), 0.5-5.0 μg/mL (r = 0.999 1), 0.15-1.50 μg/mL (r = 0.999 2), 0.25-2.50 μg/mL (r = 0.999 5), 0.6-6.0 μg/mL (r = 0.999 1), 0.45-4.50 μg/mL (r = 0.999 3), and 0.12-1.20 μg/mL (r = 0.999 4), respectively. These ten components were well resolved. Their average recoveries (n = 6) respectively were 98.7% (RSD = 0.7%), 98.0% (RSD = 1.3%), 99.6% (RSD = 1.4%), 98.0% (RSD = 1.4%), 99.1% (RSD = 1.1%), 99.4% (RSD = 0.8%), 98.8% (RSD = 0.9%), 101.1% (RSD = 0.5%), 100.6% (RSD = 0.5%), and 101.7% (RSD = 0.8%). The content of ten batches of the amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone was 0.104-0.123, 0.600-0.621, 0.501-0.523, 0.100-0.121, 0.103-0.122, 0.231-0.260, 0.043-0.065, 0.055-0.069, 0.061-0.079, 0.031-0.043 mg/g, respectively. Conclusion The method is accurate, sensitive, credible, and repeatable, which can be applied to the quality control of YQG.
ABSTRACT
Objective: To establish HPLC-DAD method for the simultaneous determination of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside in Shenqi Shiyiwei Granule (SSG). Methods: The chromatographic separation was achieved on an Waters XBridge-C18 (250 mm × 4.6 mm, 5.0 μm) column with methanol-acetonitrile-water (15:80:5) and methanol-0.1% phosphoric acid (10:90) as mobile phases for gradient elution, at the flow rate of 1.0 mL/min; The column temperature was 35℃. Results: The linear ranges of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.4-8.0 μg/mL (r = 0.999 2), 0.2-4.0 μg/mL (r = 0.999 5), 0.2-4.0 μg/mL (r = 0.999 5), 0.1-2.0 μg/mL (r = 0.999 6), 0.1-2.0 μg/mL (r = 0.999 7), 0.1-2.0 μg/mL (r = 0.999 4), 0.5-10 μg/mL (r = 0.999 2), 0.6-12 μg/mL (r = 0.999 2), 0.4-8.0 μg/mL (r = 0.999 4), 1.0-20 μg/mL (r = 0.999 6), and 0.8-16 μg/mL (r = 0.9993). The average recoveries (n = 6) were 98.1% (RSD = 0.9%), 98.1% (RSD = 1.6%), 99.1% (RSD = 1.6%), 98.3% (RSD = 1.8%), 99.5% (RSD = 1.5%), 99.9% (RSD = 0.6%), 98.5% (RSD = 0.7%), 100.4 (RSD = 0.8%), 101.6% (RSD = 0.4%), 99.7% (RSD = 0.9%), and 101.2% (RSD = 1.1%), respectively. The contents of nine batches of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.081-0.089, 0.261-0.269, 0.060-0.069, 0.038-0.047, 0.030-0.037, 0.042-0.049, 0.420-0.428, 0.141-0.151, 0.178-0.189, 0.107-0.117, and 0.069-0.078 mg/g. The results showed that there was little difference among the batches. Conclusion: The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of SSG.
ABSTRACT
Objective: To establish an HPLC-DAD method for the simultaneous determination of 10 components in Shendan Sanjie Capsule including tanshinone IIA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I. Methods: The chromatographic separation was performed on a Hypersil BDS column (150 mm × 4.6 mm, 3.5 μm) with acetonitrile-merhanol-0.1% phosphate acid solution as mobile phase at the flow rate of 1.0 mL/min for gradient elution and the column temperature was 40 ℃. The detection wavelength was set at 270 nm for tanshinone IIA, 294 nm for magnolol and honokiol, 283 nm for naringin and neohesperidin, 203 nm for ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1, 260 nm for calycosin 7-O-β-D-glucopyranoside, and 220 nm for atractylenolide I. The volume of sample injection was 10 μL. Results: Ten compounds were well separated under the determined chromatographic conditions. The RSD values of precision and repeatability experiment were all less than 2% and the sample solution was stable during 10 h. All the compounds had a wide linear range and good linearity: the linear range of tanshinone IIA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I were 112-560 μg/mL (r = 0.999 6), 64-320 μg/mL (r = 0.999 1), 48-240 μg/mL (r = 0.999 3), 80-400 μg/mL(r = 0.999 4), 80-400 μg/mL (r = 0.999 5), 16-80 μg/mL (r = 0.999 2), 16-80 μg/mL (r = 0.999 1), 16-80 μg/mL (r = 0.999 1), 40-200 μg/mL (r = 0.999 2), and 56-280 μg/mL (r = 0.999 3), respectively. The average recoveries were in the range of 98.43%-101.52% and the RSD values were all less than 2.0%. The content ranges of tanshinone IIA, magnolol, honokiol, naringin, neohesperidin, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, calycosin 7-O-β-D-glucopyranoside, and atractylenolide I in six batches of Shendan Sanjie Capsule were 0.829-0.840 mg/g, 0.538-0.548 mg/g, 0.360-0.369 mg/g, 0.210-0.219 mg/g, 0.111-0.118 mg/g, 0.081-0.089 mg/g, 0.070-0.078 mg/g, 0.111-0.117 mg/g, 0.072-0.080 mg/g, and 0.130-0.137 mg/g, respectively. Conclusion: The method is simple and convenient, the methodology validation shows that determination result of the method is accurate and reliable and it can be an effective approach for the quality control of Shendan Sanjie Capsule.