悬钩木膏提取工艺优化及质量标准研究OA

Objective:To optimize the extraction process of Rubus chingii paste and establish a quality standard protocol.Methods:An orthogonal experimental design was employed to screen the optimal extraction conditions.Extraction frequency,ex-traction time,and water volume were selected as the key factors for investigation,with dried extract yield and ellagic acid content used as the evaluation indexes.Catechin in the extract was identified using Thin-Layer Chromatography(TLC).Ellagic acid con-tent was quantified by High-Performance Liquid Chromatography(HPLC).Chromplus C18 column(5 μm,4.6 mm×250 mm)was used with the mobile phase of acetonitrile(A)and 0.1％phosphoric acid in water(B)with isocratic elution(19％A:81％B)for 30 min.The detection wavelength was set at 253 nm with the flow rate of 1.0 mL·min-1.The column temperature was 30 ℃ with the injection volume of 10 μL.Results:The optimal extraction parameters were determined as follows:water volume 12 times the raw material weight,extracted 3 times,for 60 min each time.Identification by TLC confirmed that the catechin spot in the test sample corresponded exactly to the reference standard.The HPLC method for ellagic acid quantification demonstrated excellent linearity within the range of 0.018 76 to 0.216 40 mg·mL-1(R²=0.999 9).The method exhibited satisfactory precision,repeatabil-ity,stability,and recovery(average recovery:98.09％,RSD:0.43％)which met validation requirements.Analysis of six batches showed ellagic acid contents ranging from 1.10 to 1.83 mg·g-1.Considering practical production factors,the specification limit for ellagic acid was established at 1.22 mg·g-1.Conclusion:This study provides solid evidence for the industrial-scale production and quality assessment of Rubus chingii Paste.Further multivariate analysis is needed to understand the variation in content among samples from different geographical origins.