白花香莲解毒颗粒制备工艺研究

目的 优选出白花香莲解毒颗粒的最佳制备工艺。方法 以方中主药白花蛇舌草的特异性成分去乙酰车叶草酸甲酯及出膏率为考察指标，采用正交试验方法，优选出白花香莲解毒颗粒的最佳提取工艺。以成型率、溶化性、流动性等多项指标，对辅料、用量、工艺等条件进行考察，确定处方的成型工艺。结果 白花香莲解毒颗粒的最佳提取工艺为加10倍量水，提取2次，每次1.5 h；成型工艺为按稠膏：糊精=1：2比例加入糊精，以糊精稠膏混合物0.25%的阿司帕坦和0.25%甜菊素作为矫味剂，再加入45%乙醇作为润湿剂，混匀，过14目筛制粒，80℃鼓风干燥，整粒，即得。结论 优选出的提取工艺和成型工艺稳定可行，可为白花香莲解毒颗粒的制备与生产提供参考。     

正交试验优选天钩平肝颗粒的成型工艺

目的 基于正交试验法优选天钩平肝颗粒的成型工艺。方法 以颗粒的成型率、溶化时间、流动性的综合得分为评价指标,采用L₉(3⁴)正交试验法优化药辅比、润湿剂的体积分数和用量,筛选出天钩平肝颗粒的成型工艺。结果 天钩平肝颗粒的最佳药辅比为稠膏∶糊精∶淀粉=1∶1∶1(g∶g∶g),以85%乙醇作润湿剂,润湿剂用量为润湿剂∶稠膏=74∶100(mL∶g)。结论 优选出的天钩平肝颗粒成型工艺重复性好,质量稳定可靠,为其大批量生产提供依据。     

连翘叶速溶保健茶成型工艺优选

摘 要 目的：确定连翘叶速溶保健茶的最佳成型工艺条件。方法: 以溶化性、外观、成型性为评价指标,采用单因素试验考察不同辅料与干膏粉的比例和润湿剂浓度对指标的影响,以水分为考察指标,确定干燥时间,优化最终成型工艺。结果: 最佳成型工艺：连翘叶干膏粉与乳糖的比例为1〖KG*9〗∶〖KG-*2〗1.5,混合均匀,80%乙醇为润湿剂,湿法制粒,60℃干燥1.5 h,整粒,即得。结论: 连翘叶速溶保健茶的成型工艺可行、合理,为连翘叶的综合开发利用提供参考。     

茵泽驱脂丸成型工艺优选

目的:优选茵泽驱脂丸的成型工艺.方法:以丸剂的圆整度、溶散时限、合格丸收率为评价指标,采用正交试验优选茵泽驱脂丸的最佳成型工艺.结果:其最佳工艺为以比例为20％的水作润湿剂,干浸膏和糊精的比例为1∶1.结论:优选出的成型工艺合理实用、条件可控、成品表面光滑、均匀一致、质量好.     

镇惊泻火颗粒的制备工艺研究

摘 要 目的： 研究镇惊泻火颗粒的制备工艺。方法: 采用正交试验,以干浸膏得率、甘草苷和丹酚酸B的含量为指标,对镇惊泻火颗粒的提取、纯化工艺进行研究;以合格颗粒得率为指标,对颗粒的成型工艺进行研究,优选制剂的制备工艺。结果: 铁落先煎60 min,其余各药加8倍量水,浸泡90 min,加入先煎铁落液,煎煮提取90 min,共3次。合并浓缩至相对密度1.3左右（60℃热测）,加蒸馏水至稀释比为1:2（V/V）,加乙醇至含醇量50%,24 h后滤过。滤液回收乙醇后浓缩至相对密度1.3 （60℃热测）,60℃下干燥粉碎得干浸膏。以淀粉作稀释剂,干浸膏与辅料比例1：0.8,90%乙醇为润湿剂制软材,过20目筛制粒,60℃干燥3 h,烘干,整粒,即得。结论:优选的镇惊泻火颗粒制备工艺稳定可行。     

正交试验法优选水杨酸滴丸的制备工艺

摘 要 目的：考察影响水杨酸滴丸制备的因素,确立其最佳成型工艺。方法: 考察环境因素、加热温度、基质配比与试验步骤对滴丸制备工艺的影响。以丸重差异、溶出时限及外观质量为综合评价指标,通过正交试验进一步优化滴丸的制备工艺。结果: 基质单独加热熔化后再与药液在避光密封的条件下进行混合,可防止药液迅速氧化变红。滴丸的最佳制备工艺为：聚乙二醇400与聚乙二醇6000的比例为1∶5,药液温度为50℃,滴距为8 cm,滴制速度为70滴·min^-1。结论:该工艺简单可行,制得滴丸的丸重差异、溶出时限及外观质量均符合质量要求。     

响应面法优化罗麦颗粒成型工艺的研究

摘 要 目的：优化罗麦颗粒剂的最佳成型工艺。方法: 以合格颗粒收率及吸湿性为指标对赋形剂的种类进行筛选,通过对制粒效果的考察,优选赋形剂的最佳混合比例。以合格颗粒收率、溶化性、吸湿性、感官评价的总评“归一值”作为评价指标,选取辅料倍数、乙醇浓度、柠檬酸用量为主要影响因素,采用3因素5水平中心组合设计—响应面法优化罗麦颗粒成型工艺。结果: 确定了糖粉和麦芽糊精为颗粒的赋形剂,且糖粉和麦芽糊精的最佳混合比例为3∶1。罗麦颗粒的最佳成型工艺是赋形剂用量为提取物的5倍量,润湿剂为85%乙醇,柠檬酸含量为0.3%。结论:运用中心组合设计—响应面法制备所得的罗麦颗粒具有合格收率高、吸湿性小、溶化性好、口感柔和且服用量适中等优点,表明优化罗麦颗粒湿法制粒的工艺合理、可行。     

苦参提取纯化浓缩液喷雾干燥工艺优化

摘 要 目的： 优选苦参水提纯化浓缩液喷雾干燥最佳工艺参数。方法: 采用L9(34)正交设计试验法,以浸膏粉重量及苦参碱和氧化苦参碱两者含量之和为评价指标,通过考察药液浓缩密度、进风温度、泵药速度等对苦参提取纯化浓缩液喷雾干燥工艺条件的影响。结果: 最佳喷雾干燥工艺条件为：药液密度1.07,进风温度120℃,泵药速度4 r·min^-1。结论: 该优选工艺科学、合理、稳定、可行,可为苦参提取纯化浓缩液的喷雾干燥工业化生产提供试验依据。     

糖肝煎浓缩丸水提部分的提取工艺研究

摘 要 目的：优选糖肝煎浓缩丸水提部分的提取工艺参数。方法: 以芍药苷含量和浸膏得率作为评价指标, 芍药苷含量采用高效液相色谱法,色谱条件：色谱柱:WondaSil C₁₈柱(250 mm×4.6 mm,5 μm);流动相：乙腈-0.15%磷酸溶液(16∶84);流速：1.0 ml·min^-1;柱温:30℃;检测波长：230 nm。以加水量、煎煮时间和煎煮次数作为考察因素,采用正交设计法进行方差分析优选水提取工艺参数。 结果: 优选的提取工艺为加12倍量水,提取3次,每次1 h。结论:优选的提取工艺合理、稳定、可行,为糖肝煎浓缩丸提取工艺提供了试验依据。     

正交试验优选酮通颗粒成型工艺

目的:优选酮通颗粒的成型工艺。方法:先以吸湿百分率为指标考察辅料的类别及其比例;再采用正交试验,以成型率和吸湿百分率为指标,以提取物与辅料的比例、乙醇浓度、乙醇用量为考察因素,优选成型工艺。结果:以乳糖:糊精=3:2为最佳辅料配比;最佳成型工艺为提取物与辅料按1:2的比例混匀,以70%乙醇为润湿剂制软材,乙醇用量为12%(mL·g~(-1))。成品颗粒的流动性好,临界相对湿度约为70%。结论:该成型工艺可行、稳定合理、重现性较好,可为工业化生产提供理论依据。     

对临床试验中显著性检验、区间检验及置信区间检验之间关系一致性的认识

显著性检验是最基本的统计假设检验,它的基本思想是小概率原理;区间检验是传统显著性检验的延伸,它用来检验两个总体的差异是否在某范围之内;置信区间检验是先找到药物疗效差值的置信区间,通过置信区间下限或(和)上限与界值的关系来判断两种药物非劣效、等效、优效的关系。通过公式推导发现,区间检验与显著性检验的主要区别是前者的假设中包含了有临床意义的界值△,而区间检验和置信区间检验是一致的,可以用置信区间检验实现区间检验的目的。     

谈谈两总体比较的非参数检验方法

针对不同的数据类型,探讨选用不同的非参数检验方法,并通过实例说明这些非参数检验方法的应用。     

A Comparison of Two-Sample Tests of Significance When Used With Variable Treatment Effects

This article compares the performance of many two-sample tests of significance that might be used to test the equality of means when the effect of the treatment is variable. Of the 19 tests that were compared, the normal scores test is recommended for general use in testing the null hypothesis of no treatment effect against the alternative that the distributions are stochastically ordered when the ratio of the larger standard deviation to the smaller standard deviation does not exceed 1.3. The Baumgartner-Weiß-Schindler tests and an adaptive test also have higher power than the pooled t-test, the unequal variance t-test, and the rank-sum test for many distributions. In the simulation studies, data in the first sample are generated from nine distributions, including long-tailed and skewed distributions. Data in the second sample are generated by adding a random treatment effect to a random variable that was generated from the same distribution that was used in the first sample. Because we restricted our power studies to treatment effects that are positive or zero, the population distributions will be stochastically ordered. The results of these studies demonstrate that the normal scores test is often more powerful than the t-tests and the rank-sum test. If the ratio of the standard deviations does exceed 1.3, then one of the t-tests is recommended.     

Testing equality of proportions for correlated binary data in ophthalmologic studies

In ophthalmologic studies, bilateral correlated data often arise when information involving paired organs (e.g., eyes) are measured from each subject. Adjusted chi-square approach for testing the equality of proportions has been proposed in the literature. In this article, we investigate and derive three alter- native testing procedures for the problem. Our simulation results show the score testing procedure usually produces satisfactory type I error control with higher power, and therefore is recommended. Examples from ophthalmologic studies are used to illustrate our proposed methods.     

中国药品上市后抽验模式现状及问题

目的在综合分析中国药品上市后抽验模式现状及问题的基础上,提出药品上市后抽验的建议。方法通过文献研究的方法,发现中国药品上市后抽验模式中存在的问题,并提出相关建议。结果与结论在药品抽验中引入以风险为基础的抽验模式,将药品上市后抽验结果与药品监管相衔接。     

Mutagenicity testing of quinine with submammalian and mammalian systems

Quinine hydrochloride was assayed for genotoxic activity by using 4 different test systems with distinct genetic endpoints. No indications for point mutations were observed in the Ames system. In 3 cytogenetic tests performed on small rodents, Chinese hamsters showed no genotoxic activity, while inbred strains of mice revealed a dose dependent increase of SCEs, enhanced incidence of micronuclei and elevated chromatid breaks.     

刹毒草口服液的药理作用研究

目的:研究刹毒草口服液对小鼠的药理作用。方法:用小鼠分别进行爬杆实验、炭粒廓清实验、耳肿胀实验和墨汁推进实验,观察刹毒草口服液对小鼠的抗疲劳作用、非特异性免疫功能的影响、抗炎作用和抗腹泻作用。结果:刹毒草口服液能显著延长小鼠爬杆时间,有较好的抗疲劳作用;高剂量刹毒草口服液能显著提高小鼠对惰性炭粒的吞噬指数及吞噬活性,可提高小鼠免疫功能;刹毒草口服液3个剂量组均对二甲苯致小鼠耳炎症有较好的抑制作用,且能显著降低墨汁推进的速率,有较好的抗腹泻作用。结论:刹毒草口服液具有一定抗疲劳、抗炎、提高非特异性免疫功能和抗腹泻作用。     

Simultaneous Test for Superiority and Noninferiority Hypotheses in Active-Controlled Clinical Trials∗

The primary objective of the dose-escalation trial for NGX267 was to estimate the maximally tolerated dose (MTD) and to gather detailed clinical and pharmacokinetic observations near the MTD. The MTD was defined based on the weighted average of moderate and severe adverse events. An adaptive design was employed to concentrate dosage assignments at or near the MTD. Favoring the acquisition of data near the MTD, at the expense of information at lower dosage levels, resulted in a shorter trial and no loss of the type of information required to inform subsequent studies where larger normal volunteer or patient samples are evaluated.     

氢溴酸山莨菪碱注射液细菌内毒素检查法的建立

目的:建立氢溴酸山莨菪碱注射液的细菌内毒素检查方法。方法:按《中国药典》2010年版(二部)附录相关方法确定本品细菌内毒素限值,分别进行细菌内毒素检查凝胶法和动态浊度法的干扰试验。结果:凝胶法结果表明,样品稀释2倍(5 mg/ml)时对试验无干扰作用;动态浊度法结果表明,本品稀释2倍(5 mg/ml)时外加内毒素的回收率在50%²00%之间。每1 mg氢溴酸山莨菪碱中含内毒素应小于0.35 EU。结论 :本文初步建立的氢溴酸山莨菪碱注射液细菌内毒素检查方法,可为《中国药典》增订该制剂的细菌内毒素检查项提供参考。     

Bootstrap inference in a linear equation estimated by instrumental variables

Summary We study several tests for the coefficient of the single right‐hand‐side endogenous variable in a linear equation estimated by instrumental variables. We show that writing all the test statistics—Student's t, Anderson–Rubin, the LM statistic of Kleibergen and Moreira (K), and likelihood ratio (LR)—as functions of six random quantities leads to a number of interesting results about the properties of the tests under weak‐instrument asymptotics. We then propose several new procedures for bootstrapping the three non‐exact test statistics and also a new conditional bootstrap version of the LR test. These use more efficient estimates of the parameters of the reduced‐form equation than existing procedures. When the best of these new procedures is used, both the K and conditional bootstrap LR tests have excellent performance under the null. However, power considerations suggest that the latter is probably the method of choice.