Résumé
@#An HPLC-DAD wavelength switching method(240 nm, 280 nm, 316 nm, 403 nm)was developed for simultaneous determination of seven index components: hydroxysafflor yellow A, paeoniflorin, ferulic acid, salvianolic acid B, kaempferol, formononetin and tanshinone IIA in Naoxintong capsule. The qualities of different batches of Naoxintong capsules were evaluated by statistical analysis. Seven index components in 20 batches of Naoxintong capsules were simultaneously determined by HPLC wavelength switching method with Capcell PAK C18 MG II column(250 mm × 4. 6 mm, 5. 0 μm). The mobile phase consisted of methanol-acetonitrile(25 ∶75, A)-0. 1% formic acid aqueous solution(B)with a gradient elution program and a flow rate of 1. 0 mL/min, and the column temperature was 30 °C. The results were analyzed by statistical analysis to evaluate the differences in the quality of Naoxintong capsules. Results showed that the seven active components were well separated and showed good linearity hydroxysafflor yellow A(403 nm)2. 30- 11. 50 mg/L(r=0. 999 2), paeoniflorin(240 nm)8. 81- 44. 05 mg/L(r=0. 999 6), ferulic acid(316 nm)1. 22- 6. 10 mg/L(r=0. 999 6), salvianolic acid B(280 nm)11. 61- 58. 05 mg/L(r=0. 999 4), kaempferol(403 nm)1. 16-5. 80 mg/L(r=0. 999 4), formononetin(240 nm)0. 12- 0. 60 mg/L(r=0. 999 5)and tanshinone IIA(280 nm)2. 28- 11. 40 mg/L(r=0. 999 5). The precision was good and RSD was less than 2. 0%, The repeatability was good and RSD was less than 2. 0%. The stability was good in 24 h. The average recoveries were between 97. 35%- 101. 02% and RSD was less than 2. 0%. The contents of target components in Naoxintong capsules, hydroxysafflor yellow A was 0. 213- 0. 369 mg/g, paeoniflorin was 1. 535- 3. 217 mg/g, ferulic acid was 0. 153- 0. 236 mg/g, salvianolic acid B was 2. 563- 3. 271 mg/g, kaempferol was 0. 103- 0. 181 mg/g, formononetin was 0. 022- 0. 028 mg/g, and tanshinone IIA was 0. 466- 0. 698 mg/g. HPLC wavelength change and gradient elution method was established for simultaneous determination of seven index components in Naoxintong capsule. The method is accurate, sensitive, reliable, and repeatable, and can be used for the quality control of Naoxintong capsule.
Résumé
Objective: To develop an HPLC method for the simultaneous determination of tanshinone IIA, paeoniflorin, salvianolic acid B, ferulic acid, safflor yellow A, ligustilide, and danshensu in Refined Coronary Tablets. Methods: The chromatographic separation was achieved on a Zorbax Eclipse XDB-C18 column (250 mm × 4.6 mm, 5.0 μm) with methanol-acetonitrile (25∶75, A)-0.1% formic acid (B) as mobile phases at the flow rate of 1.0 mL/min for gradient elution: 0-10.0 min, 95% B; 10.0-16.0 min, 95%-85% B; 16.0-18.0 min, 85% B; 18.0-22.0 min, 85%-75% B; 22.0-26.0 min, 75%-65% B; 26.0-40.0 min, 65%-15% B; Detection with variable wavelength: 0-19.0 min was 270 nm, 19.0-22.0 min was 230 nm, 22.0-27.0 min was 320 nm, 27.0-40.0 min was 402 nm, and the column temperature was 30 ℃. Its linear relationship, precision, repeatability, stability, and recoveries were investigated. Results: The results showed that the seven active components were well separated and showed good linearity, tanshinone IIA 0.4-8.0 mg/L (r = 0.999 5), paeoniflorin 1.2-24.0 mg/L (r = 0.999 1), salvianolic acid B 3.2-64.0 mg/L (r = 0.999 3), ferulic acid 0.08-1.60 mg/L (r = 0.999 5), safflor yellow A 1.2-24.0 mg/L (r = 0.999 3), ligustilide 0.24-4.80 mg/L (r = 0.999 7), and danshensu 0.32-6.40 mg/L (r = 0.999 7). The precision was good, and RSD was less than 2.0%. The repeatability was good, and RSD was less than 2.0%. The stability was good in 12 h. The average recoveries were between 98.05%-101.27%, and RSD was less than 2.0%. The contents of target components in Refined Coronary Tablets, tanshinone was 0.704-0.797 mg/g, paeoniflorin was 3.124-3.411 mg/g, salvianolic acid B was 7.129-7.611 mg/g, ferulic acid was 0.180-0.198 mg/g, safflor yellow A was 2.718-2.966 mg/g, ligustilide was 0.590-0.683 mg/g, and danshensu was 0.811-0.899 mg/g. Conclusion: The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of Refined Coronary Tablets.
Résumé
Objective: To develop a UPLC method for the simultaneous determination of nuciferine, psoralen, isopsoralen, tanshinone IIA, danshensu, sennoside A, sennoside B, and ursolic acid in Hedan Tablets. Methods: The chromatographic separation was achieved on an Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with methanol-acetonitrile (40:60, A)-0.1% formic acid (B) as mobile phases at the flow rate of 0.6 mL/min for gradient elution: 0-4.0 min, 90% B; 4.0-6.0 min, 90%-80% B; 6.0-9.0 min, 80%-70% B; 9.0-10.5 min, 70%-60% B; 10.5-12.0 min, 60%-50% B, 12.0-16.0 min, 50%-10% B; Detection with variable wavelength: 0-4.0 min was 215 nm, 4.0-12.0 min was 270 nm, 12.0-16.0 min was 340 nm, and the column temperature was 40°C. Its linear relationship, precision, repeatability, stability, and recoveries were investigated. Results: The results showed that the eight active components were well separated and showed good linearity. The precision was good and RSD was less than 3.0%. The repeatability was good and RSD was less than 3.0%. The stability was good in 24 h. The average recoveries were between 99.21%-101.91% and RSD was less than 3.0%. Conclusion: The method is accurate, sensitive, credible, and repeatable. It could be applied to the quality control of Hedan Tablets.