影响生物制品冻干粉针剂水分的探讨

探讨生物制品冻干粉针剂样品放置一时间后残余水分增高的原因。进行了水分测定,真空度检测,二甲硅油和丁基橡胶药用瓶塞干燥失重的检测。冻干后每只丁基橡胶药用瓶塞平均含水分0.00224g。结果表明丁基橡胶药用瓶塞灭苗,干燥和冻干过程中去除水分不彻底是引起样品中水分升高的直接原因。     

Experimental determination of viability loss of Penicillium bilaiae conidia during convective air-drying

A study was conducted on the drying of Penicillium bilaiae, a fungal micro-organism used to promote soil-bound phosphorous uptake in several crop species, such as wheat, canola and pulse crops. A wet pellet formed from a mixture of the inoculant and a starch-based carrier was air-dried to the appropriate water activity to extend the shelf-life of the viable fungal conidia. Convective air-drying was examined as a low-energy alternative to the more expensive freeze-drying technology that is currently in use. Experiments were conducted to measure the loss of conidia viability during drying in a fixed-bed, thin-layer convective dryer. The dryer air inlet temperature and relative humidity were controlled in experiments to determine the effect of thermal and dessicative stresses on conidial viability. The measured survivor fraction was determined to be dependent on solids temperature, moisture content and drying rate. Thermal stresses became significant for process temperatures above 30°C, while the survivor fraction fell sharply below a dry basis moisture ratio of 30%. Slower drying kinetics associated with high inlet air relative humidity were found to significantly improve the recovery of viable conidia. By minimising environmental stresses, survivor fractions of up to 75% could be achieved, but this result fell dramatically with the introduction of more severe conditions. A general linear statistical model is used to quantify experimental error and the significance level of each factor.     

风速对蒙古栎阔叶床层失水过程的影响

研究蒙古栎阔叶床层在近似恒温湿条件下不同风速时的失水过程,分析了风速对床层失水系数的影响.结果表明: 风速对蒙古栎阔叶床层失水过程的影响与可燃物含水率有关.从较高含水率(>75%)到近平衡含水率的多个失水过程可划分为3个阶段:有风失水速率大于无风失水速率的初始阶段、有风失水速率小于无风失水速率的中间阶段、不同风速失水速率相近的结束阶段.风速的影响随床层含水率降低而下降.蒙古栎阔叶床层的失水系数受风速、密实度和两者交互作用的影响,其中,失水系数随风速以三次多项式近似单调增加.     

Seed development in Ipomoea lacunosa (Convolvulaceae), with particular reference to anatomy of the water gap

BACKGROUND AND AIMS: Disruption of one or both of the bulges (water gap) in the seed coat adjacent to the micropyle is responsible for breaking physical dormancy (PY) in seeds of Ipomoea lacunosa and other taxa of Convolvulaceae. Hitherto, neither ontogeny of these bulges nor onset of PY together with anatomical development and maturation drying of the seed had been studied in this family. The aims of this study were to monitor physiological and anatomical changes that occur during seed development in I. lacunosa, with particular reference to ontogeny of the water gap. METHODS: Developmental anatomy (ontogeny) of seed coat and dry mass, length, moisture content, germinability and onset of seed coat impermeability to water were monitored from pollination to seed maturity. Blocking/drying and dye-tracking experiments were done to identify site of moisture loss during the final stages of seed drying. KEY RESULTS: Physiological maturity of seeds occurred 22 d after pollination (DAP), and 100 % of seeds germinated 24 DAP. Impermeability of the seed coat developed 27-30 DAP, when seed moisture content was 13 %. The hilar fissure was identified as the site of moisture loss during the final stages of seed drying. The entire seed coat developed from the two outermost layers of the integument. A transition zone, i.e. a weak margin where seed coat ruptures during dormancy break, formed between the bulge and hilar ring and seed coat away from the bulge. Sclereid cells in the transition zone were square, whereas they were elongated under the bulge. CONCLUSIONS: Although the bulge and other areas of the seed coat have the same origin, these two cell layers underwent a different series of periclinal and anticlinal divisions during bulge development (beginning a few hours after pollination) than they did during development of the seed coat away from the bulge. Further, the boundary between the square sclereids in the transition zone and the elongated ones of the bulge delineate the edge of the water gap.     

Intermittent drying of bioproducts--an overview

Unlike the conventional practice of supplying energy for batch drying processes at a constant rate, newly developed intermittent drying processes employ time-varying heat input tailored to match the drying kinetics of the material being dried. The energy required may be supplied by combining different modes of heat transfer (e.g. convection coupled with conduction or radiation or dielectric heating simultaneously or in a pre-selected sequence) in a time-varying fashion so as to provide optimal drying kinetics as well as quality of the bioproduct. This is especially important for drying of heat-sensitive materials (such as foods, pharmaceutical, neutraceutical substances, herbs, spices and herbal medicines). Intermittent heat supply is beneficial only for materials which dry primarily in the falling rate period where internal diffusion of heat and moisture controls the overall drying rate. Periods when little or no heat is supplied for drying allow the tempering period needed for the moisture and heat to diffuse within the material. As the moisture content increases at the surface of the biomaterial during the tempering period, the rate of drying is higher when heat input is resumed. It is possible to control the heat input such that the surface temperature of the product does not exceed a pre-determined value beyond which thermal damage of the material may occur. This process results in reduction in the use of thermal energy as well as the mass of air used in convective drying. Thus, the thermal efficiency of such a process is higher. The quality of the product, as such color and ascorbic acid content, is also typically superior to that obtained with a continuous supply of heat. However, in some cases, there will be a nominal increase in drying time. In the case of microwave-assisted and heat pump drying, for example, the capital cost of the drying system can also be reduced by drying in the intermittent mode.

This paper provides an overview of the basic process, selected results from experiments and mathematical models for a variety of biomaterials dried in a wide assortment of dryers. It begins with a classification of intermittent drying processes that may be applied e.g. time-varying temperature, air flow rate, operating pressure as well as heat input by different modes and in different temporal variations. The beneficial effects of improving the quality of dried bioproducts by different intermittent processes are also included and discussed.     

Effect of viscoelastic relaxation on moisture transport in foods. Part II: Sorption and drying of soybeans

The general fluid transport equation presented in Part-I of this paper is used for predicting moisture transport and viscoelastic stresses during sorption and drying of soybeans. Predicted drying curves were validated using experimental data obtained from literature (average absolute difference 6-13%). For drying temperatures used in the soybean processing industry (70–93 °C), smooth moisture profiles were obtained, which indicated Fickian (Darcian) transport. As the drying temperature approached the glass transition temperature (25 °C at 10% moisture content), the moisture profiles became sharper, which indicated non-Fickian (non-Darcian) transport. The viscoelastic stress profiles clearly exhibited the role of the force terms during imbibition and drying. Increase in drying temperature tends to decrease the stress relaxation function but reduction in moisture content during drying tends to increase it. The increase in stress due to the reduction in moisture content below 10% was not compensated by an increase in drying temperature. Drying of soybeans below 10% moisture content should be avoided in the industry because this will lead to thicker flakes that reduce the amount of oil recovery. During imbibition of soybeans, a high magnitude of stresses was obtained in the rubbery regions, which may cause critical regions prone to fissuring. The role of glass transition on stress development and critical region development was clearly observed during drying and imbibition of soybeans.Revised version: 5 October 2003     

Freeze drying of histocompatibility typing sera.

This report describes a unit employed for the freeze drying of histocompatibility typing serum using a 50-hr cycle. This unit will process approximately 3200 3-ml vials with a final residual moisture content of less than 2%. The system employs dry ice-alcohol cooled circulating baths to maintain the condensers below ?60 °C, and two shelf cooling baths to maintain the product at required temperatures during the freeze drying process.The results of a 5-yr study of the effect of residual moisture as a function of time and storage temperature is also included. Studies conducted to date indicate that with residual moistures below 2%, freeze dried histocompatibility sera can be stored at +4 °C without the loss of significant tissue typing factors. Solubility of all serum was lost when stored at +37 °C or higher during this same 5-year period.     

Acute seasonal drought does not permanently alter mass loss and nitrogen dynamics during decomposition of red maple (Acer rubrum L.) litter

Litter decomposition is a major component of nutrient cycling in forest ecosystems and is known to be sensitive to both temperature and moisture. A drought during periods of the year when moisture is normally abundant may impact decomposition more than moisture limitation during seasons that are routinely dry. We excluded precipitation for a 3‐month period during each of four seasons and measured mass loss and nitrogen (N) dynamics in Acer rubrum leaf litter by using a litterbag approach. We hypothesized that rainfall exclusion would retard mass loss during the exclusion period, with the maximum effect occurring during the spring and summer months when moisture was normally adequate and temperatures optimum for decomposition, and that exclusion during these two periods would have the greatest impact on subsequent timing of decomposition events, particularly N mineralization. Mass loss in litterbags was initially reduced by precipitation exclusion in the spring treatment only. For each season, a set of bags exposed to drying in the same way and allowed to remain in the field under ambient conditions for an additional 9 months no longer showed a difference in mass loss relative to control bags. Nitrogen accumulation was immediately and significantly reduced in the exclusion treatments in all seasons; however, like mass loss, there was no difference 9 months later. We conclude that short‐term effects of drought do occur, especially with regard to N accumulation, and that these effects do not persist and are unlikely to have any substantial effect on nutrient cycling.     

Nitrogenous fertilizer transformations in the sudan Gezira soil

Summary and Conclusions Direct measurements were made of losses of ammonia during the transformation of urea and ammonium sulphate, surface-applied to alkaline Gezira soil in containers incubated in the field, under different rates of nitrogen application and moisture conditions.The highest rate of ammonia loss occurred during the first week after application with both fertilizers, thereafter decreasing to lower values. The cumulative ammonia loss was higher with higher application of nitrogen. Ammonium sulphate gave consistently higher ammonia losses than urea and losses from open soil system were generally less than from soil in polythene bags.With lowest irrigation level used, ammonia loss attained a sizeable value throughout the incubation period with both fertilizers. With the higher moisture levels, the magnitude of ammonia loss decreased appreciably, much more so with urea than with ammonium sulphate. Induced drying and rewetting prolonged the duration of loss and increased the magnitude of cumulative loss. An appreciable loss of ammonia may take place from fertillzed Gezira Soil under warm conditions, low moisture levels and high fertilizer concentration; this may be the case with patchy fertilizer distribution and frequent light showers during early summer. It is advisable to apply the urea or ammonium sulphate when conditions are most favourable for nitrification.     

Embryo Water Status and Survival in the Recalcitrant Species Quercus robur L: Evidence for a Critical Moisture Content

The responses of Q. robur L. fruits, seeds and embryonic axesto desiccation are characterized and discussed in relation tocurrent knowledge of recalcitrant seed behaviour. A relationshipbetween viability and seed moisture content is described. Thisrelationship was unaffected by rate of drying, year of harvestor presence of the pericarp. Desiccation sensitivity did notincrease with storage. Excised embryonic axes survived to lower moisture contents thanintact seeds. However, in the intact seed, loss of viabilityappeared to be determined by a critical moisture content inthe cotyledons. Consequently, the level of desiccation tolerancewithin the axis attached to cotyledons was not determined byaxis drying rate. A link is drawn between the difference in the desiccation toleranceof embryonic axes and of cotyledons, and estimates of theirdifferent levels of matrix-bound water. The results presentedare consistent with a critical moisture content for survivalwhich is determined by the loss of all free cellular water.This hypothesis takes account of the differential desiccationsensitivity of seed tissues and differences in desiccation tolerancebetween species.     

Using a Mass Balance to Determine the Potency Loss during the Production of a Pharmaceutical Blend

The manufacture of a blend containing the active pharmaceutical ingredient (API) and inert excipients is a precursor for the production of most pharmaceutical capsules and tablets. However, if there is a net water gain or preferential loss of API during production, the potency of the final drug product may be less than the target value. We use a mass balance to predict the mean potency loss during the production of a blend via wet granulation and fluidized bed drying. The result is an explicit analytical equation for the change in blend potency a function of net water gain, solids losses (both regular and high-potency), and the fraction of excipients added extragranularly. This model predicts that each 1% gain in moisture content (as determined by a loss on drying test) will decrease the API concentration of the final blend at least 1% LC. The effect of pre-blend solid losses increases with their degree of superpotency. This work supports Quality by Design by providing a rational method to set the process design space to minimize blend potency losses. When an overage is necessary, the model can help justify it by providing a quantitative, first-principles understanding of the sources of potency loss. The analysis is applicable to other manufacturing processes where the primary sources of potency loss are net water gain and/or mass losses.     

Optimization of the Secondary Drying Step in Freeze Drying Using TDLAS Technology

The secondary drying phase in freeze drying is mostly developed on a trial-and-error basis due to the lack of appropriate noninvasive process analyzers. This study describes for the first time the application of Tunable Diode Laser Absorption Spectroscopy, a spectroscopic and noninvasive sensor for monitoring secondary drying in laboratory-scale freeze drying with the overall purpose of targeting intermediate moisture contents in the product. Bovine serum albumin/sucrose mixtures were used as a model system to imitate high concentrated antibody formulations. First, the rate of water desorption during secondary drying at constant product temperatures (−22°C, −10°C, and 0°C) was investigated for three different shelf temperatures. Residual moisture contents of sampled vials were determined by Karl Fischer titration. An equilibration step was implemented to ensure homogeneous distribution of moisture (within 1%) in all vials. The residual moisture revealed a linear relationship to the water desorption rate for different temperatures, allowing the evaluation of an anchor point from noninvasive flow rate measurements without removal of samples from the freeze dryer. The accuracy of mass flow integration from this anchor point was found to be about 0.5%. In a second step, the concept was successfully tested in a confirmation experiment. Here, good agreement was found for the initial moisture content (anchor point) and the subsequent monitoring and targeting of intermediate moisture contents. The present approach for monitoring secondary drying indicated great potential to find wider application in sterile operations on production scale in pharmaceutical freeze drying.     

The rapid and long-lasting growth of grasses following small falls of rain on stony downs in the arid interior of Australia

Abstract Stony downs consist of grassy areas that alternate with areas that have a substantial stone cover. The stone-covered areas are impermeable, and most rain falling on them runs off, substantially increasing the effective rainfall in adjacent grassy areas. As a result, 20–25 mm of rain on stony downs wetted the soil around the grass to a depth of 140–170 mm and allowed sustained grass response. This is much less than the 35–40 mm of rain required for the same response on red clay or grey clay plains. Grasses respond very rapidly after rain. Some have green shoots the day after rain, and all have responded by the second day. Ephemerals dry off in 4–6 weeks, but most tussock grasses still have some green foliage 8–10 weeks after rain. Deeper rooted tussock grasses remain green for so long because most of the moisture that reaches deeper roots after rain remains there. Most moisture loss is through the soil surface and is recognizable as a drying front that descends through the soil profile. Soil above the drying front is nearly air dry (<5% moisture) while soil below the front has substantial moisture (14–16%). By about a month after rain in summer, the drying front is at a depth of about 80–120 mm. This is near the tips of the roots of ephemeral grasses and the ephemerals then dry off rapidly. Only the tips of the leaves of deep rooted grasses like Mitchell grass (Astrebla spp.) dry off. Their leaves continue to remain mostly green during most of the second month after rain and they do not dry off completely until the third month when the drying front reaches the bottom of the main root system.     

Changes in root hydraulic conductivity for two tropical epiphytic cacti as soil moisture varies

The tropical epiphytic cacti Epiphyllum phyllanthus and Rhipsalis baccifera experience extreme variations in soil moisture due to limited soil volumes and episodic rainfalls. To examine possible root rectification, whereby water uptake from a wet soil occurs readily but water loss to a dry soil is minimal, responses of root hydraulic conductivity (L_p) to soil drying and rewetting were investigated along with the underlying anatomical changes. After 30 d of soil drying, L_p decreased 50%–70% for roots of both species, primarily because increased suberization of the periderm reduced radial conductivity. Sheaths composed of soil particles, root hairs, and mucilage covered young roots and helped reduce root desiccation. Axial (xylem) conductance increased during drying due to vessel differentiation and maturation, and drought-induced embolism was relatively low. Within 4 d of rewetting, L_p for roots of both species attained predrought values; radial conductivity increased for young roots due to the growth of new branch roots initiated during drying and for older roots due to the development of radial breaks in the periderm. The decreases in L_p during drought reduced plant water loss to a dry soil, and yet maximal water uptake and transpiration occurred within a few days of rewetting, helping these epiphytes to take advantage of episodic rainfalls in a moist tropical forest.     

Preservation of Bacteria by Circulating-Gas Freeze Drying

Water-washed Serratia marcescens and Escherichia coli were freeze dried in a circulating-gas system at atmospheric pressure. This convective procedure resulted in a substantially higher survival of organisms than could be obtained by the vacuum method of freeze drying. There was little or no decrease in cell viability during convective drying when the residual moisture content was 15% or higher. Below this level, survival declined with decreasing moisture content. A detailed comparison of the convective and vacuum methods indicated that the advantage gained by freeze drying bacteria in air accrues in the early period of sublimation, at which time cells were found to be sensitive to vacuum drying but insensitive to air drying. An explanation for this difference is proposed, based upon the kinetics of water removal in the two processes. In brief, it is suggested that the convective method permits samples to be dried more uniformly; and regional over-drying, which may be deleterious even if transient, is thus avoided in achieving the optimal level of moisture.     

Fluid bed drying of guarana (Paullinia cupana HBK) extract: Effect of process factors on caffeine content

The aim of this study was to study the convective drying of the hydroalcoholic extracts obtained from powdered guarana seeds in a spouted bed dryer. The influence of process variables, such as the convective airflow rate, extract feed rate, and air inlet temperature, on the quality of the dry extract was determined using the caffeine and moisture content for the process evaluation. The caffeine content in the alcoholic and dried extracts was determined by capillary gas chromatography. The experiments were performed following a 3³ factorial design and the data analyzed by response surface. The analysis of dry extract showed that the air and extract feed rates did not significantly affect (25% level) the caffeine content, but that drying temperature is a major factor to consider when the extract is submitted to fluid bed drying. Caffeine losses were significant (1% level) for drying temperatures above 120°C, while moisture content was lower than 3% for temperatures above 120°C. The data showed that there is an optimum temperature for the drying of guarana extracts in spouted beds, and under the conditions used in this study it was 120°C.     

The Development of Desiccation-tolerance and Maximum Seed Quality During Seed Maturation in Six Grain Legumes

‘Physiological maturity’, i.e. the time when seedsreach their maximum dry weight during development, occurredwhen maturation drying on the parent plant in the field hadreduced seed moisture content to approximately 60 per cent infaba bean (Vicia faba L.), lentil (Lens culinaris Medic.), chickpea(Cicer arietinum L.), white lupin (Lupinus albus L.), soya bean(Glycine max [L.] Merr.) and pea (Pisum sativum L.) The onsetof desiccation-tolerance, i.e. the ability of seeds to germinatefollowing harvest and rapid artificial drying, coincided withphysiological maturity, except in pea where it occurred a littleearlier at about 70 per cent moisture content. Maximum seedquality as determined by maximum viability, minimum seedlingabnormalities and maximum seedling size occurred in pea, chickpeaand lupin when seeds were harvested for rapid drying at physiologicalmaturity; but for maximum seed quality in the other speciesmaturation drying had to proceed further - to about 45 per centmoisture content in soya bean and to about 30 per cent moisturecontent in lentil and faba bean seed crops. Much of this variationamongst the six species, however, was due to differences inthe variation in maturity within each seed crop. Results forindividual pods showed that peak maturity, i.e. maximum seedquality following harvest and rapid artificial drying, was achievedin all six species once maturation drying had reduced the moisturecontent of the seeds to 45–50 per cent. In pea, faba beanand soya bean there was a substantial decline in viability andan increase in seedling abnormalities when harvest was delayedbeyond the optimal moisture content for harvest.     

A theoretical expression for drying time of thin lumber

An analytical expression for the drying time of thin lumber is derived, based on a method presented in this study. The laws of moisture content change in wood as function of mass transfer are used for the theoretical approach. The diffusion equation for moisture content is set up for a three-dimensional block of lumber based on the assumption of uniform initial distribution of moisture throughout the specimen. The boundary condition stipulates that the moisture gradient at the boundary is proportional to the deviation of the moisture content of the slab from the equilibrium value at that temperature. These conditions are used to derive an analytical expression for the time required to get from an initial moisture distribution to a desired final moisture content of thin lumber. For a sample calculation, the result of drying time agrees within 10% with the prediction of previously published analytical formulas for the drying curve.     

Determination of End Point of Primary Drying in Freeze-Drying Process Control

Freeze-drying is a relatively expensive process requiring long processing time, and hence one of the key objectives during freeze-drying process development is to minimize the primary drying time, which is the longest of the three steps in freeze-drying. However, increasing the shelf temperature into secondary drying before all of the ice is removed from the product will likely cause collapse or eutectic melt. Thus, from product quality as well as process economics standpoint, it is very critical to detect the end of primary drying. Experiments were conducted with 5% mannitol and 5% sucrose as model systems. The apparent end point of primary drying was determined by comparative pressure measurement (i.e., Pirani vs. MKS Baratron), dew point, Lyotrack (gas plasma spectroscopy), water concentration from tunable diode laser absorption spectroscopy, condenser pressure, pressure rise test (manometric temperature measurement or variations of this method), and product thermocouples. Vials were pulled out from the drying chamber using a sample thief during late primary and early secondary drying to determine percent residual moisture either gravimetrically or by Karl Fischer, and the cake structure was determined visually for melt-back, collapse, and retention of cake structure at the apparent end point of primary drying (i.e., onset, midpoint, and offset). By far, the Pirani is the best choice of the methods tested for evaluation of the end point of primary drying. Also, it is a batch technique, which is cheap, steam sterilizable, and easy to install without requiring any modification to the existing dryer.