ABSTRACT
Objective: To establish HPLC coupled with wavelength switching and gradient elution method (HPLC-DVD) for simultaneous determination of nine main components (α-cyperone, genipin-1-β-D-gentiobioside, geniposide, crocin I, senkyunolide H, senkyunolide I, senkyunolide A, ligustilide, and atractylodin) in Yueju Tablets. Methods: The chromatographic separation was achieved on Zorbax Eclipse Plus C18 (250 mm × 4.6 mm, 5 μm) column with methanol-acetonitrile (2∶1) (A)-0.2% glacial acetic acid solution (B) as mobile phases for gradient elution, at the flow rate of 0.9 mL/min; The detection wavelength was set at 240 nm for α-cyperone, genipin-1-β-D-gentiobioside and geniposide, 440 nm for crocin I, 280 nm for senkyunolide H, senkyunolide I, senkyunolide A and ligustilide, and 340 nm for atractylodin. The volume of sample injection was 10 μL. Results: The nine active components were well separated and showed good linearity, such as α-cyperone 2.58—51.60 μg/mL (r = 0.999 4), genipin-1-β-D- gentiobioside 11.99—239.80 μg/mL (r = 0.999 9), geniposide 17.96—359.20 μg/mL (r = 0.999 6), crocin-I 3.98—79.60 μg/mL (r = 0.999 7), senkyunolide H 2.82—56.40 μg/mL (r = 0.999 9), senkyunolide I 2.38—47.60 μg/mL (r = 0.999 9), senkyunolide A 6.04—120.80 μg/mL(r = 0.999 5), ligustilide 7.98—159.60 μg/mL (r = 0.999 3), and atractylodin 6.51—130.20 μg/mL (r = 0.999 2). The precision was good, and RSD was not more than 1.22%. The repeatability was good, and RSD was not more than 1.75%. The stability was good in 18 h, and RSD was not more than 1.37%. The average recoveries and corresponding RSD values were 97.64% (0.98%), 99.09% (1.46%), 100.11% (1.03%), 97.87% (0.80%), 98.59% (1.19%), 96.89% (1.34%), 99.38% (0.58%), 98.50% (1.22%), and 99.71% (0.85%), respectively. The contents of 10 batches of α-cyperone, genipin-1-β-D-gentiobioside, geniposide, crocin I, senkyunolide, H, senkyunolide I, senkyunolide A, ligustilide and atractylodin were 0.282—0.344, 2.099—2.445, 3.628—4.225, 0.758—0.913, 0.241—0.286, 0.217—0.266, 1.077—1.291, 1.386—1.623, and 1.137—1.434 mg/tablet. Conclusion: HPLC coupled with wavelength switching and gradient elution method has been established for simultaneous determination of nine components in Yueju Tablets. The method is simple, quick, accurate, and it can be used for content determination and quality control of Yueju Tablets.
ABSTRACT
Objective: To establish the batch release criteria of Gardenia jasminoides intermediate purification process based on statistical process control technology in order to ensure the batch-to-batch consistency and stability. Methods: Forty-eight batches of G. jasminoides intermediate purified solution were collected as the calibration set. The content of chlorogenic acid, shanzhiside, geniposidic acid, deacetyl asperulosidic acid methyl ester, genipin-1-β-D-gentiobioside, geniposide, and total acid were determined to establish the quantitative release criteria. Near-infrared spectra (NIRS) were acquired to establish the qualitative release criteria. Seventeen batches of G. jasminoides intermediate purified solution were prepared under different process conditions by the Box-Behnken experimental design. They were regarded as the validation set to verify the feasibility of the established quantitative and qualitative release criteria. Results: The established quantitative release ranges were: chlorogenic acid 5.753-6.713 mg/g, shanzhiside 9.456-10.723 mg/g, geniposidic acid 3.313-4.401 mg/g, deacetyl asperulosidic acid methyl ester 15.260-16.419 mg/g, genipin-1-β-D-gentiobioside 30.529-33.473 mg/g, geniposide 165.17-175.16 mg/g, and total acid 45.028-53.118 mg/g, respectively. The established qualitative release upper limits were: Hotelling T2 = 4.067 8 and DModX = 1.218 8. For sample 1, 5, 7, 9, 10, 14-17 from the validation set, the content of quality control indicators satisfied the quantitative release criteria and NIRS satisfied the qualitative release criteria. Conclusion: Based on NIRS and statistical process control technology, the developed quantitative and qualitative release criteria are simple and feasible. They could be used for the production quality control of G. jasminoides intermediate purification process.