酿酒用粮食中淀粉快速检测方法的研究与应用

中国白酒是以高粱、玉米、小麦、大米及糯米等高淀粉含量的粮食为原料,经多道工序酿制而成。原料淀粉含量的多少直接影响出酒率。为有效缩短粮食淀粉含量的检测时间,减少操作过程中的人为误差,建立了检测淀粉含量的快速方法。样品前处理采用微波快速消解代替冷凝回流酸水解,加快淀粉水解速度、控制水解完全;样品检测采用快速检测仪代替人工微沸滴定,提高了实验操作的重复性和易用性。应用该方法检测多种酿酒用粮食的淀粉含量,并与国家标准方法GB 5009.9—2016的检测结果进行对比,两种方法的测定结果之间无显著性差异。结果显示,淀粉快速检测方法能够适用于多种酿酒用粮中总淀粉含量的检测,大大缩短检测时间,减少人为操作误差,重复性和再现性良好,线性回归及相关性系数≥0.999 7。     

高温高压-酸水解-液相法测定薯类食品中的淀粉含量

以土豆为原料，采用高温高压-酸水解-液相法对土豆中的淀粉含量进行测定，以期为食品中淀粉含量的测定提供高效、准确的方法。研究结果表明，较优水解条件为：盐酸浓度3.9 mol/L,消解时间35 min,消解温度109℃;在此条件下，样品中淀粉可完全水解。采用液相色谱法进行测定，结果与国标法大致相同。与常规酸水解-滴定法比较，该方法具有水解时间短，操作简便，测定结果准确，重复性好等优点，是一种可行的测定方法。     

高效液相色谱法测定烟草中的淀粉含量

研究了用高效液相色谱法测定烟草中的淀粉含量,即先用酸将烟草中的淀粉水解为葡萄糖,再以甘露醇为内标物,用WatersSugar Pak1钙型阳离子交换柱为固定相,0 05g/LEDTA钙钠水溶液为流动相,示差折光仪为检测器测定淀粉水解产生的葡萄糖含量,由葡萄糖含量换算为淀粉含量。该方法的检测限为1 0mg/L,相对标准偏差为1 6%～2 1%,标准回收率在95%～105%之间。并用该方法测定了几种烟草样品中的淀粉含量。     

酸水解-斐林试剂滴定法测定大米淀粉含量的研究

本实验利用酸水解-斐林试剂滴定法测定不同地区大米淀粉含量,并与DNS比色法及GB/T 5009.9-2008酸水解法的测定结果进行对比,对该方法的测定准确性进行研究。结果表明,酸水解-斐林试剂滴定法与国标法测定结果相近,滴定法的标准差与相对标准偏差均小于0.1,DNS比色法测定结果较低,且标准差与相对标准偏差均远远高于国标法与本法。显著性比较中,本法与国标法间差别不显著,DNS比色法与国标法和本法差异均显著。回收率实验中,国标法、滴定法和DNS比色法平均回收率分别是99.68%、99.14%、100.06%。说明本法具有较高的稳定性和准确性,且测定结果精密度好,是大米淀粉含量测定的一种简单有效的方法。     

酸酶水解-HPLC法检测香菇多糖中β-D-葡聚糖含量

为了更有效地监控食品和医药行业中香菇多糖制品的质量,建立了一种香菇多糖中主要活性成分β-D-葡聚糖含量测定的新方法:香菇多糖样品经酸部分水解后用β-1,3-葡聚糖外切酶和β-葡糖苷酶进一步完全水解以测定总葡聚糖含量;另用淀粉葡萄糖苷酶水解样品中α-葡聚糖;根据HPLC测定的总葡聚糖与α-葡聚糖含量之差计得β-D-葡聚糖含量。分别用该方法和苯酚硫酸法及刚果红法测定已知含量的β-D-葡聚糖对照样品的结果表明:该方法最接近于对照品标示值,且重复性好,可用作为香菇多糖产品中β-D-葡聚糖含量测定的专属方法。     

甘薯中淀粉测定方法的比较与优化

淀粉含量的测定方法多种多样,但是关于甘薯淀粉的测定方法,目前尚无统一标准。本研究通过对甘薯干基获得方式,淀粉水解方式以及还原糖测定方式三个主要因素对甘薯淀粉含量测定结果的影响进行探究。实验发现,冷冻干燥样品测定的淀粉质量分数比高温干燥样品显著高出38.43%,酸水解方式比酶水解显著高出6.51%。还原糖测定方法中,DNS1和DNS2测定方法分别比斐林试剂滴定法显著高出29.67%和9.47%,DNS1比DNS2测定方法显著高出20.04%。不同水解-还原糖测定方法纯淀粉回收率和加标淀粉回收率均处于95%~105%之间,变异系数均小于2%,准确度和精确度符合质控规范。综合分析表明,冷冻干燥酶水解DNS1法测定甘薯淀粉含量具有最高的准确性和精确性,冷冻干燥酸水解DNS2法则具有最佳的实用性和方便性。     

不同脱脂方法对大米直链淀粉含量测定结果的影响

直链淀粉含量是大米的重要品质指标,国家标准规定采用甲醇回流抽提法脱脂检测.本研究采用浸提法脱脂与抽提法脱脂进行对比分析,探究不同脱脂方法对大米直链淀粉含量测定结果的影响.结果表明,采用甲醇回流抽提法脱脂比甲醇浸提法脱脂测得的直链淀粉含量数值高,说明采用浸提法脱脂脂类物质去除不完全,原因是直链淀粉和淀粉颗粒中的脂质形成复...     

超声波-湿热法结合酸水解制备大米抗性淀粉及其理化性质研究

研究了超声波-湿热法结合酸水解制备大米RS3的最佳工艺条件。探讨了超声波-湿热法过程中淀粉的含水量、反应温度、反应时间以及酸水解过程中的柠檬酸浓度、加热时间、老化时间对大米RS3得率的影响,通过单因素实验和正交实验,确定了超声波-湿热法制备RS3的最佳工艺条件:大米淀粉的含水率30%、处理温度130℃、处理时间为10 h,RS3得率为32.173%;在此基础上结合酸水解的最佳工艺条件为:柠檬酸的浓度0.15 mol/L、加热时间为20 min、老化时间24 h,RS3的得率为40.672%。并对这两种最佳工艺条件下所制备的大米RS3的物理化学性质进行表征。结果表明,超声波-湿热法结合酸水解所制备的RS3内部结构更为致密,水分子不易进入,含水量、溶解性、膨润力最小,热稳定性相对较好,在偏光显微镜下呈现良好的分散性,说明采用超声波-湿热法结合酸水解所制备的RS3具有更好的理化性质。     

黄变对大米酸水解的影响

本文通过对正常大米和黄变米(Postharvest yellowing of rice,PHY)进行硫酸水解处理,分别用0.1、0.5、1.0 mol/L的硫酸溶液浸泡样品72 h,并测定酸水解前后样品的热力学性质、结晶性质以及表观结构特性,研究样品之间结构的差异。结果显示,黄变过程导致大米酸水解后的热特性发生改变,表现为糊化温度范围的减小,在1 mol/L硫酸条件下,籼米黄变米的糊化温度范围为45.64 ℃,籼米正常米的糊化温度范围是61.26 ℃,粳米黄变米的糊化温度范围为47.46 ℃,粳米正常米的糊化温度范围为50.95 ℃;X射线衍射(XRD)和小角X射线散射(SAXS)的结果表明,硫酸水解大米之后,大米内部直链淀粉无定形背景区和支链淀粉非晶层均被破坏,且酸溶液浓度越高,大米内部的无定形区被破坏的越明显。在1.0 mol/L的硫酸溶液处理时,黄变样品的结晶层发生重排,结构趋于有序化;观察表观结构表明黄变米在经过酸水解后,比普通大米相比具有更松散的结构形态。     

基于GC-MS的粳稻谷糙米大米挥发性成分差异性研究

本文应用GC-MS技术,对同一储藏期(90 d)、不同储藏条件下的粳稻谷,其稻谷、糙米、大米3种不同形式样品中挥发性成分进行测定,用主成分分析法(PCA)研究不同样品间挥发性成分的差异,进行比较分析,并运用离子流图谱对分析结果准确性进行验证。结果表明,稻谷、糙米、大米样品中的挥发性物质分别有150、125、98种,挥发性物质种类大致相同,主要有7类:烷烃类、苯烯烃类、醛类、醇类、酮类、酸酯类、杂环类,其中贡献率较大的是烷烃类、苯烯烃类、酸酯类和酮类,贡献率大小顺序依次为烷烃类酸酯类苯烯烃类酮类。稻谷中酮类物质作用最明显,大米中烷烃类物质作用最明显,而糙米中7类物质作用水平基本相当。糙米与大米中挥发性成分受温度与水分影响较大,而稻谷则相对稳定,从挥发性成分稳定性方面考虑,在流通领域中,稻谷加工产品糙米和大米不宜长期储存。     

酸解时间对大米淀粉结构性质的影响

以4种不同直链淀粉含量的大米淀粉(0%的优糯3号、10.90%的稻花灿、21.03%的聚两优、28.46%的华优香占)为原料,酸解处理不同时间,以酸解大米淀粉的酸解率、颗粒形貌、结晶性质、溶解度的变化为指标衡量不同酸解时间对大米淀粉结构及性质的影响。结果表明,不同直链淀粉含量的大米淀粉具有不同的耐酸性,酸解时间对不同直链淀粉含量大米淀粉的结构和性质有着不同的影响。大米淀粉酸解率与直链淀粉含量成反比,优糯3号为50%而华优香占仅为30%;所有淀粉颗粒在酸解后均产生一定程度的破碎,偏光十字变形直至消失,酸解相同时间,直链淀粉含量高的大米淀粉破碎率低;酸解未改变淀粉的晶型,仍为A晶型;随着酸解时间的延长相对结晶度增加;淀粉的溶解度随着酸解时间的增加而增大。     

湿热处理对糯米粉血糖生成指数值及相关指标的影响

利用湿热处理工艺降低糯米粉血糖生成指数（glycemic index,GI）值,并对相关指标进行比较研究。通过水分含量、温度、处理时间对糯米粉直链淀粉含量和消化特性的影响,确定单因素范围,然后采用Box-Behnken设计,以直链淀粉含量（和GI值显著负相关）为指标,优化了糯米粉湿热处理工艺。最后将最优工艺所得的糯米粉（HMT）和普通糯米粉（WR）、仅进行酶解后的糯米粉（ER）进行体外消化特性和GI值的对比研究,以分析湿热处理对糯米粉GI值的影响。研究表明,经优化的最佳湿热处理时间为2.3 h、湿热处理温度为116 ℃、水分含量为20%,在优化条件下糯米粉直链淀粉含量为3.62%±0.01%,实测值均值与理论值（3.62%）一致,表明该模型可用于优化糯米粉湿热处理工艺。最优条件下制备的糯米粉快消化淀粉（rapidly digestible starch, RDS）含量下降,慢消化淀粉（slowly digestible starch, SDS）和抗消化淀粉（resistant starch, RS）含量上升;水解指数（hydrolysis index）明显降低,同时GI值降低30.1%。该法制备的糯米粉具有较低的GI值,可为低GI糯米粉开发的进一步研发提供实验思路。     

Ordered structure and thermal property of acid-modified high-amylose rice starch

High-amylose cereal starch has a great benefit on human health. Acid modification is very helpful for application of high-amylose starch in food and non-food industries. In this study, the ordered structure of acid-modified high-amylose rice starch was investigated by GPC, HPAEC, ¹³C CP/MAS NMR and XRD. Acid preferentially degraded the amylose, then A chain and short B chain of amylopectin. Relative double helix content and crystallinity both initially increased sharply and then progressively with acid hydrolysis. The relative crystallinity of starches obtained from ¹³C CP/MAS NMR was higher than that from XRD. The onset gelatinisation temperature decreased, while the peak and conclusion temperatures increased with increasing hydrolysis time. The endothermic value initially increased and then decreased with acid hydrolysis. The swelling power decreased while solubility increased after acid hydrolysis. These results add to our understanding of the effect of acid hydrolysis on the high-amylose rice starch.     

Characterization and Utilization of Acid‐modified Rice Starches for Use in Pharmaceutical Tablet Compression

Acid modified, agglomerated starches offer specific advantages as fillers in production of pharmaceutical tablets. Spray drying can improve processing of tablet mixtures significantly. In order to investigate prerequisites in utilization of rice starch, non‐waxy and waxy types were partially hydrolyzed in 6% (w/v) HCl solution at room temperature for varied length of time to obtain rice starches with increased crystallinity (so‐called crystalline rice starches). Scanning electron micrographs of native and highly crystalline starches were used to study the morphological changes and to suggest the mode of acid attack during hydrolysis. Exo‐corrosion distributed over the surface of acid‐modified waxy rice starch (AWRS) was observed after 192 h of hydrolysis. In contrast, the surface of acid‐modified rice starch (ARS) remained unchanged at 192 h of acid hydrolysis. The amylose content and the median particle size (diameter) were reduced with increasing hydrolysis time. It was found by X‐ray diffraction that the relative crystallinity of acid‐modified starches at >95% relative humidity was clearly increased with prolonged hydrolysis time. For studying tablet properties spherical agglomerates of the native and acid modified starches were directly compressed at 4 kN to obtain tablets. Crushing strength and disintegration time of tablets increased with relative crystallinity. In contrast, tablet friability was reduced. Concerning tablet functionality, the crystalline starches were positioned in overlapping ranges between the common commercial tablet fillers (microcrystalline cellulose, pregelatinized starch and lactose, respectively).     

湿热及酶解处理对糯米粉体外消化特性和血糖生成指数的影响

目的 研究酶解处理、湿热处理和湿热复合酶解处理对糯米粉体外消化特性和血糖生成指数(glycemic index, GI)的影响。方法 采用体外消化法测定了不同处理糯米粉的水解度和血糖生成指数值, 并通过X-射线衍射和激光共焦拉曼光谱实验测定了不同处理糯米的淀粉晶体结构。结果 3种处理的水解度和抗性淀粉(resistant starch, RS)相对含量增加, 慢消化淀粉(slowly digestible starch, SDS)相对含量降低; 其中湿热复合酶解处理条件下, RS相对含量最高, 为71.31%; 酶解处理条件下, RS相对含量最低, 为67.66%。酶解处理、湿热处理和湿热复合酶解处理的GI值分别为79.1、76.0和70.6。3种处理后糯米淀粉的晶体结构发生改变, 3种处理均使分子短程有序度与结晶度增加, 其中湿热复合酶解处理条件下, 结晶度最高, 为34.41%。 结论 湿热复合酶解处理后的糯米粉抗消化特性增强且GI值降低, 湿热复合酶解工艺可能通过影响糯米粉的体外消化率来降低GI值。     

Morphology and physicochemical changes in rice flour during rice paper production

Rice flour samples from four steps of rice paper processing were prepared from rice grain, Chainart 1 variety: wet-milled flour (WMF), 24 hour soak-milled flour (24SF), 48 hour soak-milled (48SF), and dried rice paper (DRP). Decrease in protein, fat and amylose content occurred during prolonged fermentation but increase of ash content due to addition of salt occurred. Because of lactic acid bacteria activity, increases occurred in titratable acidity as lactic acid in soaking water during fermentation. Scanning electron microscopy revealed that starch granule surfaces wilted and showed corrosion channels with longer fermentation. Pasting and thermal properties of the four samples were significantly different; 24SF and 48SF showed lower peak viscosity, breakdown and final viscosity. Increasing fermentation time increased gelatinization temperature, endothermic energy and relative crystallinity. The results suggest that lactic acid and enzyme hydrolysis during fermentation in rice paper processing caused significant decrease in amorphous structure and increase in crystallinity in rice starch.     

大米抗性辛烯基琥珀酸淀粉酯的制备及特性分析

为探究抗性淀粉制备新途径,提高大米特别是碎米资源的利用价值,以大米淀粉为原料,水相法制备大米辛烯基琥珀酸淀粉酯（OSA淀粉）,以取代度DS和反应效率RE为考察指标,探讨反应温度、反应pH、酸酐滴加时间和淀粉浆浓度对DS和RE的影响。对OSA淀粉进行湿热处理,探究湿热处理时间对抗性淀粉含量和理化特性的影响,并进行体外消化试验。结果表明:制备OSA淀粉适合的工艺条件为反应温度40 ℃、反应pH为9.0、酸酐滴加时间为4 h、淀粉乳浓度30%,此条件下得到的OSA淀粉DS为1.3915,RE为78.2%。将此条件获得的OSA淀粉湿热处理18 h,抗性淀粉含量从25.2%增加至42.2%。在模拟胃肠道中消化水解率为58.8%。     

Comparative Studies on Some Physico-chemical, Thermal, Morphological, and Pasting Properties of Acid-thinned Jicama and Maize Starches

Comparative studies on acid hydrolysis of jicama and maize starch were carried out using concentrations of hydrochloric acid of 1.5%, 3.0%, and 4.5% (w/v), for 3 and 6 h, at 40°C. Native maize and jicama starches showed important morphological, thermal, and structural differences from those of tubers and cereals which potentially offer diverse industrial applications. Jicama starch showed low amylose content (12%) and small size of starch granules. Due to these characteristics, jicama starch was more susceptible to degradation during hydrolysis process than maize starch. Under the experimental conditions employed, the acid degradation was not particularly severe, as shown by scanning electronic microscopy analysis which showed small degraded zones and similar X-ray patterns in both starches. However, jicama starch was more susceptible to acid hydrolysis than maize starch, as revealed by the considerable increase in water solubility index, damaged starch, and crystallinity values. Also, the higher susceptibility of jicama starch than maize starch to the hydrolysis conditions was reflected in the sugar content release during hydrolysis. The relative crystallinity of hydrolyzed maize starches decreased during hydrolysis, while those of hydrolyzed jicama starches increased attributable to the lower amylose content of jicama starch in relation to maize starch. Maize and jicama hydrolyzed starches showed low viscosity values with relation to their native starch counterparts. However, native jicama starch showed lower viscosity values than maize starch, suggesting a lower internal stability of the starch granules during hydrolysis. Both native and hydrolyzed maize starches showed higher enthalpy, T _o, T _p, and T _c values than jicama starch and the broadening of the endotherms decreased during the hydrolysis of both starches.     

稻谷实仓储藏品质变化规律研究

稻谷在实仓储藏过程中的品质变化对其食用及商业价值具有重要影响,本试验以浙江省级粮库中不同储藏年份的早籼稻为研究对象,分别测定了其发芽率、电导率、丙二醛含量、蛋白质组分、淀粉含量、脂肪酸值、脂肪酸组分以及挥发性成分等与稻谷品质密切相关的重要指标。结果显示,随着仓储时间的增加,稻谷的发芽率显著降低;电导率和脂肪酸值则呈上升趋势,丙二醛含量无显著变化;蛋白质含量与淀粉含量随时间变化相对较小,但受稻谷品种的影响较大;脂肪酸组分以油酸、亚油酸和棕榈酸为主,其含量变化呈逐步上升趋势;挥发性成分中酯类化合物含量呈先下降后上升趋势,醛类物质与此相反,烷烃类无显著变化,烯类和醇类物质呈上升趋势,酮类物质则呈下降趋势。上述结果表明,随着仓储时间的延长,稻谷的生命活力逐步下降、细胞膜受到损坏、脂质氧化并产生不良风味,可根据这些指标的变化情况初步判断稻谷品质的劣变程度,并为稻谷实仓储藏的条件控制与优化提供一定的理论依据。     

Hydrolysis of wheat starch and its effect on the Falling Number procedure: experimental observations†

The underlying mechanisms of starch hydrolysis in cereal grains, as measured by the Falling Number procedure, were studied. Wheat starch, spiked with barley malt α‐amylase, was used as a model experimental system. A non‐invasive and real‐time monitoring system was developed to simultaneously record the sample temperature and stirrer velocity profiles, which are critical parameters that affect Falling Number readings. Experimental results show that the repeatability of the Falling Number procedure can be improved by slowing the heating rate, which is accomplished by increasing the quantity of sample components (ie starch and water) while maintaining the same proportion as currently specified in standard methodology. Among the tested range of heating rates, the best repeatability of Falling Number readings was obtained with 8.4 g starch and 30.0 g water. The experimental findings of this study also serve as basic information for the development of mathematical models on the hydrolysis of starch. © 1999 Society of Chemical Industry