不同干燥工艺的六味地黄提取物的粉体学性能评价

目的考察不同干燥工艺对六味地黄提取物物理性质与粉体学性质的影响。方法选用六味地黄提取物考察了真空干燥、喷雾干燥及冷冻干燥对六味地黄提取物物理性质与粉体学性质的差异。结果六味地黄喷雾干燥所得浸膏粉的黏性较小,所得粉粒较细小、圆整,且压缩度、抗张强度、吸湿速率及平衡吸湿量均比真空干燥的大。冷冻干燥所得浸膏粉的比表面积、孔容均比真空干燥的大。结论干燥方式及原理的不同导致了干燥产物物理性质与粉体学性质的差异,应根据不同制备的需求选择不同的制备工艺。     

不同干燥方式对中药提取物粉体学性质的影响

目的：考察不同干燥方式对复方中药舒胸片方提取物粉体学性质的影响。方法以真空干燥、微波真空干燥及喷雾干燥三种方法,探讨不同干燥方式对复方中药舒胸片方提取物粉体学性质的差异。结果三者中真空干燥产物流动性最好,微波真空干燥产物的平衡吸湿量最小,喷雾干燥所得圆整性好、粒匀,压缩成型性较优。结论干燥工艺不同导致了干燥产物粉体学性质的差异,各粉体学性质之间存在一定的相关性。     

不同干燥方式对杜仲叶4种活性成分含量的影响

目的:考察不同干燥方式对杜仲叶中活性成分含量的影响,为建立杜仲叶在产地采收后的干燥加工方式提供参考。方法:取杜仲叶采用不同干燥方法[自然阴干72 h、自然晒干36 h、烘干(60℃6 h、80℃2 h、100℃1 h、120℃0.5 h)、微波真空冷冻干燥12 h、真空冷冻干燥12 h]对杜仲叶进行处理;采用高效液相色谱法同时测定样品中桃叶珊瑚苷、京尼平苷酸、绿原酸、京尼平苷的含量,并与未处理的鲜品进行比较。结果:2种冷冻干燥后的样品与鲜品中的4种成分含量接近,并高于其他干燥方式处理的样品。结论:干燥方法对杜仲叶有效成分具有较显著的影响,微波真空冷冻干燥和真空冷冻干燥较自然阴干、自然晒干、烘干更能保留杜仲鲜叶中的活性成分。     

荷叶提取物不同干燥工艺对总黄酮含量的影响

目的:考察荷叶乙醇提取液不同干燥方式对总黄酮含量的影响.方法:分别采用常压干燥、减压干燥、喷雾干燥、冷冻干燥及红外干燥的方式对荷叶乙醇提取液进行干燥处理,采用紫外分光光度法对不同干燥方式所得干膏总黄酮进行含量测定.并进行方差分析.结果:各干燥方式对荷叶总黄酮含量影响无显著性差异.结论:不同干燥方式对荷叶干膏中总黄酮含量影响不大,其中红外干燥方式所需的成本最低、效率最高.     

干燥方式对大血藤提取物粉体学性质的影响

目的考察不同干燥方式对大血藤提取物的粉体学性质的影响,并初步筛选适宜的粉体表面改性剂。方法考察了真空干燥、喷雾干燥两种方法对大血藤提取物的粉体学性质的影响,并通过粉体表面改性技术,初步筛选了改性剂。结果喷雾干燥法所制的大血藤浸膏粉粒径小而均匀,圆整性好,吸湿性及流动性略逊于真空干燥制品,大血藤浸膏粉经过微晶纤维素改性后流动性、吸湿性及成形性得到明显改善。结论干燥方式的不同导致了干燥产物粉体学性质的差异,通过粉体表面改性技术可以改善中药提取物的粉体学性质。     

干燥工艺对黄芪桂枝五物汤粉体的物理指纹图谱和有效成分影响研究

目的： 考察干燥工艺对黄芪桂枝五物汤粉体的物理指纹图谱和有效成分含量的影响,优选出最佳干燥方法。方法： 采用冷冻干燥、真空干燥和喷雾干燥法制备粉体,以5个一级指标和11个二级指标构建物理指纹图谱,并测定其有效成分（黄芪甲苷、毛蕊异黄酮葡萄糖苷、芍药苷、肉桂酸、总多糖）含量。通过11个二级指标评价粉体学性质,建立相应的物理指纹图谱;采用相似度评价和主成分分析法对比其物理指纹图谱;通过计算可压性参数评价粉体的压缩成型性。结果： 3种粉体的有效成分含量无显著性差异（P>0.05）。3种粉体均具有较好的可压性、较差的稳定性和流动性,其中喷雾干燥具有良好的均一性,冷冻干燥和真空干燥具有良好的堆积性。3种干燥工艺的物理指纹图谱相似度75.5%~95.4%。结论： 干燥工艺对黄芪桂枝五物汤物理指纹图谱影响较大,以喷雾干燥为最佳。     

不同干燥方法对红花中有效成分的影响

目的比较不同干燥方法对红花提取物中有效成分羟基红花黄色素A的影响。方法采用高效液相色谱法测定红花各干燥产物中羟基红花黄色素A的含量,以其为指标,对不同干燥方法进行考察。结果采用真空干燥,喷雾干燥,冷冻干燥所得的产物中羟基红花黄色素A的含量分别为3.21%,8.55%,8.20%。结论相比真空干燥,喷雾干燥和冷冻干燥更适于红花提取物的干燥。     

消炎去脂片不同工艺制备过程中指标成分含量变化研究

目的 考察消炎去脂片不同工艺制备过程中指标成分含量变化情况.方法 分别采用真空干燥、微波干燥对组方提取、浓缩制备的流浸膏进行干燥,制得干浸膏,再分别加辅料制备成颗粒,采用喷雾干燥制粒法将流浸膏直接喷雾干燥制粒,超高效液相色谱法(UPLC)检测消炎去脂片干浸膏、成品颗粒中黄芩苷和栀子苷的含量,考察真空干燥、微波干燥和喷雾干燥及制粒过程对指标成分含量变化的影响.结果 以组方中指标成分含量为指标,真空干燥含量均最低,喷雾干燥与微波干燥相近或互有高低.制粒、烘干过程对黄芩苷含量影响较大,而对栀子苷含量影响不大.结论 不同干燥方法及制粒、烘干工艺对中药制剂制备过程中指标成分含量均有影响,实际工艺研究中必须进行有效的筛选.     

蒸制断生后真空冷冻干燥对天麻质量的影响

目的:提高真空冷冻干燥天麻的天麻素含量。方法:采用蒸制后再真空冷冻干燥的方法对天麻进行干燥,考察天麻的外观及微观结构,测定天麻复水率、多糖和天麻素含量及不同干燥工艺下天麻粉末在模拟胃肠液中的溶出量与溶出率。结果:与鲜天麻直接真空冷冻干燥相比,天麻经蒸制后再真空冷冻干燥其外观和切面微观结构无显著变化。95℃蒸制4 min后再真空冷冻干燥,其天麻素含量和复水率分别为0.875%和502%,显著高于鲜天麻直接冷冻干燥(0.280%和362%)和120℃蒸制4 min后再真空冷冻干燥(0.775%和466%),但3个干燥工艺下天麻的多糖含量无显著差异。热风干燥天麻及真空冷冻干燥天麻粉末的红外指纹图谱谱峰位置相近,峰形相似,说明天麻成分无显著变化。不同工艺干燥天麻的天麻素在模拟胃液和肠液中的溶出率无显著差异。结论:天麻经95℃蒸制4 min后再进行真空冷冻干燥可在保持其外观和微观形态的条件下显著提高天麻素含量和复水率,天麻真空冷冻干燥生产中可对该工艺进行适当修正以推广应用。     

指纹图谱技术评价不同干燥方式对地龙氨基酸组分提取物的影响

目的 对不同干燥方式所得地龙氨基酸组分提取物进行指纹图谱测定方法的研究, 比较不同干燥方式对地龙氨基酸组分提取物品质的影响。方法 采用异硫氰酸苯酯柱前衍生化反相高效液相色谱法, 测定并比较真空冷冻干燥、真空减压干燥和微波干燥3种方式所得地龙干燥样品以及未经干燥样品的指纹图谱, 以中药色谱指纹图谱相似度评价系统计算相似度, 并进行图谱比较和指认分析。结果 建立了不同干燥技术处理的地龙氨基酸组分提取物高效液相指纹图谱, 确定了17个共有峰, 同一干燥方法不同批次干燥产品的镜像度较高, 具有良好的相似性(>0.9), 不同干燥方法所得提取物之间有较大的质量差异。结论 HPLC指纹图谱分析法可较全面的反映不同干燥技术处理的地龙氨基酸组分提取物间的差异, 可用于同类提取物干燥工艺的质量控制和工艺评价。冷冻干燥法是地龙氨基酸组分提取物最适宜的干燥方法。     

不同干燥方法对丹参毛状根有效成分含量及其抗氧化活性的影响

目的：探讨不同干燥方法对丹参毛状根中主要化学成分含量及其抗氧化活性的影响,尤其关注采后干燥对丹参毛状根酚酸类成分是否也有类似对植物根一样的胁迫诱导作用。方法丹参毛状根经冷冻干燥、真空干燥、阴干和晒干四种不同干燥方式处理后,采用高效液相色谱法测定毛状根中包括9种酚酸类和4种酮类成分的含量;利用1,1-二苯基-2-三硝基苯肼（ DPPH）自由基清除试验、超氧阴离子清除试验、脂质过氧化抑制试验测定毛状根提取物的抗氧化活性。结果与冷冻干燥相比,真空干燥和阴干对酚酸类成分的影响不大,但酮类成分下降约50％;晒干处理后二类成分均严重损失达90％左右;晒干样品提取物抗氧化活性也显著下降。结论冷冻干燥是最适合丹参毛状根的干燥方法;与丹参根不同,采后干燥对毛状根的酚酸类成分无诱导作用。     

The impact of drying method and formulation on the physical properties and stability of methionyl human growth hormone in the amorphous solid state

The objective of this work was to investigate the impact of drying method and formulation on the physical stability (aggregation) and selected important physical properties of dried methionyl human growth hormone (Met-hGH) formulations. Solutions of Met-hGH with different stabilizers were dried by different methods (freeze drying, spray drying, and film drying), with and without surfactant. Properties of the dried powders included powder morphology, specific surface area (SSA), protein surface coverage, thermal analysis, and protein secondary structure. Storage stability of Met-hGH in different formulations was also studied at 50 degrees C and at 60 degrees C for 3 months. The dried powders displayed different morphologies, depending mainly on the method of drying and on the presence or absence of surfactant. Film dried powders had the lowest SSA (approximately 0.03 m(2)/g) and the lowest total protein surface accumulation (approximately 0.003%). Surfactant caused a reduction in the SSA of both spray dried and freeze dried powders. Spray dried powders showed greater protein surface coverage and SSA relative to the same formulations dried by other means. Greater in-process perturbations of protein secondary structure were observed with polymer excipients. Formulation impacted physical stability. In general, low molecular weight stabilizers provided better stability. For example, the aggregation rate at 50 degrees C of Met-hGH in a freeze dried trehalose-based formulation was approximately four times smaller than the corresponding Ficoll-70-based formulation. Drying method also influenced physical stability. In general, the film dried preparations studied showed superior stability to preparations dried by other methods, especially those formulations employing low molecular weight stabilizers.     

地黄叶总苷浸膏真空带式干燥工艺优化研究

目的研究地黄叶总苷浸膏真空带式干燥的最佳工艺,并与其他干燥方法进行比较。方法以干燥产品含水率及有效成分保留率为评价指标,对影响干燥效果的因素进行考察。在单因素实验结果的基础上,采用L9（34）正交试验法,结合方差分析与多指标综合评分结果,获得地黄叶总苷浸膏真空带式干燥的最佳工艺参数,并将其干燥效果与真空烘箱干燥、微波真空干燥进行比较。结果地黄叶总苷浸膏真空带式干燥的最佳工艺条件为传送带速度4cm·min-1,浸膏进料速度25mL·min-1,加热系统温度75℃,75℃,该条件下地黄叶总苷浸膏干燥产物含水率为2.54%,毛蕊花糖苷保留率和地黄叶总苷保留率分别为94.54%和90.49%。结论优选得到的地黄叶总苷浸膏真空带式干燥工艺稳定可靠。与真空烘箱干燥和微波真空干燥相比,真空带式干燥具有干燥产品含水率低、有效成分保留率高、干燥时间短和可连续生产等优点,为中药浸膏的真空带式干燥工艺设计和过程控制提供了参考。     

不同干燥技术对金银花质量的影响

目的研究不同干燥技术对金银花质量的影响。方法采用晒干、烘干、微波干燥、真空干燥4种干燥技术对大白期金银花花蕾外观性状、有效成分及营养成分进行分析研究。结果经微波干燥、真空干燥处理的金银花中绿原酸含量较高,可溶性糖含量以晒干处理的最高,游离氨基酸含量以真空干燥处理的最高。结论不同干燥技术对金银花有效成分和营养成分的影响是不同的,金银花作为药材使用时,应首先选择能最大保持药效成分的方法进行加工,可能的情况下再兼顾营养成分。     

不同工艺干燥的玄参中桃叶珊瑚苷含量比较

目的 建立测定玄参中桃叶珊瑚苷含量的高效液相色谱法,探讨不同干燥工艺对玄参质量的影响.方法 分别对鲜玄参进行自然晾晒干燥、烘箱干燥和微波真空干燥;采用Kromasil C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(5:95),检测波长为206 nm,柱温为30℃,流速为1.0 mL/min.结果 桃叶珊瑚苷进样量在0.11～1.81 μg与峰面积呈良好线性关系(r=0.999 7,n=6);采用微波真空干燥和自然晾晒干燥的玄参中桃叶珊瑚苷含量远高于烘箱干燥的玄参.结论 高效液相色谱法测定玄参中桃叶珊瑚苷含量,方法专属性好、准确、稳定可靠.微波真空技术用于中药玄参的干燥,不仅工艺简单、干燥时间短,而且能较好地保留桃叶珊瑚苷等有效成分.     

Drying-Induced Variations in Physico-Chemical Properties of Amorphous Pharmaceuticals and Their Impact on Stability II: Stability of a Vaccine

Objectives To investigate the impact of drying method on the storage stability of dried vaccine formulations. Materials and Methods A sucrose-based formulation of a live attenuated virus vaccine of a parainfluenza strain, with and without surfactant, was dried from by different methods; freeze drying, spray drying and foam drying. Dried powders were characterized by differential scanning calorimetry, specific surface area (SSA) analysis and by electron spectroscopy for chemical analysis (ESCA) to evaluate vaccine surface coverage in the dried formulations. Dried formulations were subjected to storage stability studies at 4, 25 and 37°C. The vaccine was assayed initially and at different time points to measure virus-cell infectivity, and the degradation rate constant of the vaccine in different dried preparations was determined. Results SSA was highest with the spray dried preparation without surfactant (∼ 2.8 m²/g) and lowest in the foam dried preparations (with or without surfactant) (∼ 0.1 m²/g). Vaccine surface coverage was estimated based on ESCA measurements of nitrogen content. It was predicted to be highest in the spray dried preparation without surfactant and lowest in the foam with surfactant. Stability studies conducted at 25°C and 37°C showed that the vaccine was most stable in the foam dried preparation with surfactant and least stable in spray dried preparations without surfactant and in all freeze dried preparations regardless of the presence of surfactant. Addition of surfactant did lower the SSA and vaccine surface coverage in freeze dried preparations but still did not improve storage stability. Conclusions In drying methods that did not involve a freezing step, good storage stability of Medi 534 vaccine in the dried form was found with low SSA and low vaccine surface accumulation, both of which integrate into low fraction of vaccine at the surface. Ice appears to be a major destabilizing influence.     

Radio Frequency - Assisted Ultrasonic Spray Freeze Drying for Pharmaceutical Protein Solids

This study examined physical stability of spray freeze dried (SFD) bovine serum albumin (BSA) solids produced using the radio frequency (RF)-assisted drying technique. BSA formulations were prepared with varying concentrations of trehalose and mannitol, using an excipient-free formulation as control. These formulations were produced using either traditional ultrasonic spray freeze drying (SFD) or RF-assisted ultrasonic spray freeze drying (RFSFD). The dried formulations were then characterized using Karl Fischer moisture content measurement, powder X-ray diffraction (PXRD), size exclusion chromatography (SEC), and solid-state hydrogen/deuterium exchange with mass spectrometry (ssHDX-MS). Moisture content did not have a good correlation with the physical stability of the formulations measured by SEC. ssHDX-MS metrics such as deconvoluted peak areas of the deuterated samples showed a satisfactory correlation (R² = 0.914) with the SEC stability data. RFSFD improved the stability of formulations with 20 mg/ml of trehalose and no mannitol, and had similar stability with all other formulations as compared to SFD. This study demonstrated that RFSFD technique can significantly reduce the duration of primary drying cycle from 48.0 h to 27.5 h while maintaining or improving protein physical stability as compared to traditional lyophilization.