改性壳聚糖复合膜的制备及优化

以壳聚糖为原料经改性制备的巯基化壳聚糖为成膜基质,再添加结冷胶、甘油、氯化钙和纳他霉素,通过流延成膜制备复合膜。以膜的拉伸强度、断裂伸长率、水蒸汽透过率以及透光率为考查指标,对结冷胶、甘油、氯化钙和纳他霉素进行单因素实验,然后通过Plackett-Burman（PB）试验和最陡爬坡试验确定对膜拉伸强度影响显著的因素以及最佳试验范围。最后以拉伸强度为评价指标进行响应面试验,得出二次响应预测模型,优化出了复合膜的最佳配比。结果表明:单一壳聚糖膜拉伸强度为0.928 MPa,但断裂伸长率仅为5.91%;单一巯基化壳聚糖膜拉伸强度仅为0.350 MPa,断裂伸长率为14.47%。当基础膜液中巯基化壳聚糖0.20 g,改性条件为结冷胶0.18 g,甘油1.00 g,氯化钙0.17 g,纳他霉素0.01 g时,复合膜的拉伸强度最大,达到4.986±0.087 MPa;改性壳聚糖复合膜的拉伸强度得到显著提高（P<0.05）。本研究结果为改性壳聚糖复合膜的制备、复合膜综合性能提高以及在食品保鲜领域的应用提供理论支撑。     

“Vitamin E” fortified parenteral lipid emulsions: Plackett–Burman screening of primary process and composition parameters

The objective of this study was to screen the effect of eight formulations and process parameters on the physical attributes and stability of “Vitamin E”-rich parenteral lipid emulsions. Screening was performed using a 12-run, 8-factor, 2-level Plackett–Burman design. This design was employed to construct polynomial equations that identified the magnitude and direction of the linear effect of homogenization pressure, number of homogenization cycles, primary and secondary emulsifiers, pre-homogenization temperature, oil loading, and ratio of vitamin E to medium-chain triglycerides (MCT) in the oil phase on particle size, polydispersity index, short-term stability, and outlet temperature of manufactured emulsions. The viscosity of vitamin E was reduced from 3700 (100%) to 64 mPa.s (30%) by MCT addition. As viscosity is critical for efficient emulsification, vitamin/MCT ratio was the most significant contributor for the stability of emulsions. Particle size increased from 236 to 388 nm, and percentage vitamin remaining emulsified after 48 h dropped from 100 to 73% with increase in vitamin/MCT ratio from 30/70 to 70/30. Significant decrease in particle size and PI, and an increase in outlet temperature were also observed with increase in homogenization pressure and number of homogenization cycles. Emulsifiers and oil loading, however, had insignificant effect on the responses. Overall, stable submicron emulsions at vitamin/MCT ratio of 30/70 could be prepared at 25,000 psi and 25 cycles in ambient conditions. The identification of these parameters by a well-constructed design demonstrated the utility of screening studies in the “Quality by Design” approach to pharmaceutical product development.     

海洋平台环境设计参数的Plackett Copula分布估计

利用Plackett Copula分别构造波高、风速及流速的二维及三维概率分布,并用单变量设计法、条件分布众值及均值法及三维联合重现期法获得三个荷载变量的不同组合,计算导管架平台的基底剪力,利用三维概率分布估计变量组合的联合重现期。对结果比较分析可知,单变量设计法所得剪力值远远大于其他方法所得剪力值,其独立分布所得重现期远远大于联合变量的重现期。条件分布所得剪力值的大小取决于主变量的选择。计算表明,波高对剪力的影响最大,当以波高为主值利用条件分布进行计算时,其剪力值最大。以风速、流速为主值的工况,所得平台基底剪力小。利用三维Plackett Copula构造三维联合分布进行平台设计参数的估计,考虑了变量之间的相关性,与传统的单变量法相比,所得设计环境条件数值减小,将使平台建设成本降低,适用于边际油田的开发。     

Split-Plot Experiments with Unusual Numbers of Subplot Runs

In many experimental situations, it may not be feasible or even possible to run experiments in a completely randomized fashion as usually recommended. Under these circumstances, split-plot experiments in which certain factors are changed less frequently than the others are often used. Most of the literature on split-plot designs is based on 2-level factorials. For those designs, the number of subplots is a power of 2. There may however be some situations where for cost purposes or physical constraints, we may need to have unusual number of subplots such as 3, 5, 6, etc. In this article, we explore this issue and provide some examples based on the Plackett and Burman designs. Also algorithmically constructed D-optimal split-plot designs are compared to those based on Plackett and Burman designs.     

A New Class of Supersaturated Designs

Supersaturated designs are useful in situations in which the number of active factors is very small compared to the total number of factors being considered. In this article, a new class of supersaturated designs is constructed using half fractions of Hadamard matrices. When a Hadamard matrix of order N is used, such a design can investigate up to N – 2 factors in N/2 runs. Results are given for N ≤ 60. Extension to larger N is straightforward. These designs are superior to other existing supersaturated designs and are easy to construct. An example with real data is used to illustrate the ideas.     

Implementation of quality by design approach in manufacturing process optimization of dry granulated,immediate release,coated tablets – a case study

The aim of this study was to optimize the process of tablets compression and identification of film-coating critical process parameters (CPPs) affecting critical quality attributes (CQAs) using quality by design (QbD) approach. Design of experiment (DOE) and regression methods were employed to investigate hardness, disintegration time, and thickness of uncoated tablets depending on slugging and tableting compression force (CPPs). Plackett–Burman experimental design was applied to identify critical coating process parameters among selected ones that is: drying and preheating time, atomization air pressure, spray rate, air volume, inlet air temperature, and drum pressure that may influence the hardness and disintegration time of coated tablets. As a result of the research, design space was established to facilitate an in-depth understanding of existing relationship between CPPs and CQAs of intermediate product (uncoated tablets). Screening revealed that spray rate and inlet air temperature are two most important factors that affect the hardness of coated tablets. Simultaneously, none of the tested coating factors have influence on disintegration time. The observation was confirmed by conducting film coating of pilot size batches.     

橡胶籽蛋白提取工艺研究

研究了碱提酸沉法提取橡胶籽蛋白的工艺条件,通过Plackett Burman试验设计筛选出对橡胶籽蛋白提取有显著影响的因素为pH、提取温度和料液比.在单因素试验的基础上,采用响应面法优化,得到最佳工艺条件为:碱提pH9.8,提取温度57.7℃,料液比1∶43.5,酸沉pH 4.4.在最佳工艺条件下,橡胶籽蛋白提取率达70.64％,纯度为83.56％.     

Production of organic solvent tolerant lipase by Staphylococcus caseolyticus EX17 using raw glycerol as substrate

BACKGROUND: In this work we used Plackett–Burman statistical design and central composite design in order to optimize culture conditions for lipase production by Staphylococcus caseolyticus strain EX17 growing on raw glycerol, which was obtained as a by‐product of the enzymatic synthesis of biodiesel. The stability of lipase was verified over several organic solvents, such as methanol, ethanol and n‐hexane. RESULTS: Optimal culture conditions for lipase production were found to be 36 °C, initial pH 8.12, glycerol 30 g L^?1, olive oil 3.0 g L^?1, and soybean oil 2.5 g L^?1, with 145.8 U L^?1 of enzyme activity. When commercial glycerol was substituted by the raw glycerol from biodiesel synthesis, lipolytic activity was 127.3 U L^?1. Experimental validation of enzyme production matched values predicted by the mathematical model, which was 138.3 U L^?1. Stability tests showed that lipase from S. caseolyticus EX17 was stable in methanol, ethanol, and n‐hexane. CONCLUSIONS: Results obtained in this work suggest that raw glycerol can be used for lipase production by S. caseolyticus EX17 and that this enzyme has a potential application in the synthesis of biodiesel. Copyright © 2008 Society of Chemical Industry