Definitive screening design combined with design space for optimizing purification process of Scutellariae Radix extract / 中国中药杂志

In the pharmacopoeia, many process parameters for the purification process of Scutellariae Radix are unclear. In this study, deterministic screening design combined with design space method was used to optimize the purification process of Scutellariae Radix extract. Nine method parameters such as mass fraction of solution(X_1), first acid precipitation pH(X_2) and first holding time(X_3) in the purification process were firstly studied by definitive screening design. The yield of baicalin was defined as the evaluation index. A stepwise regression method was used then to build quantitative models between evaluation index and method parameters and the three most critical impact parameters were determined. Probability-based design space was calculated and successfully verified with the experimental error simulation method. Finally, the second standing temperature, the first standing temperature and the pH value of the second acid precipitation were determined as the three most critical method parameters. The recommended operating space was as follows: the second standing temperature 5-7 ℃, the first standing temperature 13-15 ℃, and the pH of the second acid precipitation 1.5-1.7. Within this operating space, the baicalin yield in the purification process was over 80%, and the probability of reaching the standard was over 0.96. In this study, we optimized the effect of various parameters for the purification process of the Scutellariae Radix extract in the pharmacopoeia on the yield of baicalin and provided a reference for industrial production of the exact of Scutellariae Radix.

Quantitative chromatographic fingerprint analysis of Sanye Tangzhiqing Decoction based on quality by design concept / 中国中药杂志

In this work,a high performance liquid chromatography-ultraviolet( HPLC-UV) detection technology was used to establish fingerprint analysis method for Sanye Tangzhiqing Decoction following an analytical quality by design( AQb D) approach. Firstly,column temperature,flow rate,and gradient elution conditions were determined as the method parameters needing to be optimized. Then according to the results of definitive screening design,three critical method attributes( CMAs) were identified,including peak number,the percentage of common peak area to total peak area,and retention time of the last peak. A stepwise regression method was used then to build quantitative models between CMAs and method parameters. Probability-based design space was calculated and successfully verified using the experimental error simulation method. After the analysis conditions were optimized,the contents of six components,namely chlorogenic acid,paeoniflorin,rutin,hyperoside,quercetin-3-O-β-D-glucuronide,and salvianolic acid B were simultaneously determined. There were 19 common peaks in the fingerprint and their common peak area accounted for 96% of the total peak area. Both fingerprint and quantitative analysis methods were validated applicable in methodology study,and they can be applied to determine new samples.

Spray Drying of Pequi Pulp: Process Performance and Physicochemical and Nutritional Properties of the Powdered Pulp

The objective of this work was to optimize the spray drying of pequi pulp using maltodextrin as carrier agent and Tween 80 as surfactant agent. A central composite rotatable design was used to evaluate the influence of inlet air temperature (140 to 200°C), maltodextrin (15 to 30%) and surfactant (0 to 5%) concentration on the process performance and physicochemical and nutritional properties of the dried powdered pulp. The dependent variables were process yield (27.4 - 51.7%), outlet air temperature (106.5 - 135°C), energetic efficiency (29.9 - 44.8%), moisture content (0.25 - 1.43%), water activity (0.09 to 0.21), hygroscopicity (9.1 - 12.1 g adsorbed moisture/100g dry matter), vitamin C content (129.8 - 303.0 mg/g solids pequi) and total carotenoids content (8.2 - 94.9 mg carotenoids/g solids pequi). The spray drying of pequi pulp was optimized for maximum vitamin C and total carotenoids content using response surface methodology, which were attained at 152°C, surfactant concentration of 1% and maltodextrin concentration of 18%. The characterization of the pequi pulp powder obtained at the optimized condition evaluating the particles sizes, bulk density and porosity. The morphology showed spherical and smooth particles with several sizes.