微波消解-原子荧光光谱法测定脐橙果皮、果肉中的硒

在微波消解仪中以硝酸和过氧化氢为消解液对脐橙果皮、果肉进行消解,在10％硝酸介质条件下,采用原子荧光光谱仪测定脐橙果皮、果肉中的硒.并用此方法对不同地区脐橙果皮、果肉检出含硒量进行分析. 该方法检出限为0.001μg/ml,回收率为97.84％～103.54％,相对标准偏差为1.52％～3.28％.方法试剂简单,污染少,操作简单、快速,是测定脐橙中硒含量的好方法.     

苹果、脐橙中铅和汞的快速测定的方法研究

研究一种简单快速测定苹果和脐橙中铅和汞的方法。在铁氰化钾-酒石酸体系下,用微波消解-原子荧光光谱法快速测定铅和汞的含量。结果表明:在优化的工作条件下,铅和汞的线性范围分别为0~100μg/L和0~2.00μg/mL,检出限分别为0.37μg/L和4.64×10-3μg/L,加标回收率为98.5%和97.1%,相对标准偏差均小于5%(n=11)。该方法具有操作简便、快速、灵敏度高的优点,可作为苹果和脐橙中微量铅和汞快速测定的方法。     

电感耦合等离子体原子发射光谱法同时测定江西脐橙中多种微量元素

采用硝酸-高氯酸对江西赣南8个县所产的脐橙样品进行消解,电感耦合等离子体原子发射光谱法(ICP-AES)同时测定试样中Al、As、Ba、B、Ca、Co、Cr、Cu、Fe、K、Li、Mg、Mn、Ni、P、Pb、Zn、Be、Cd、Se、Sr、La、Ce、Y、Sm、Lu等元素的含量。该法的相对标准偏差为0.42%～4.51%,加标回收率为87.7%～114.1%。实验结果表明:脐橙中含有丰富的K、Ca、P和Mg,不同县所产的脐橙各种微量元素含量存在一定差异。     

赣南稀土矿区果园土壤和脐橙中稀土元素含量的测定

针对赣南稀土矿区脐橙果园土壤及脐橙,研究表层土壤及土壤中稀土元素的赋存形态,并测定脐橙中稀土元素的含量。土壤样品经HNO3-HF-HClO4 酸体系预消解后再经微波消解,然后用电感耦合等离子体质谱(ICPMS)测定其中15 种稀土元素含量。为进一步研究土壤中稀土元素的赋存形态,土壤样品经连续提取法(BCR)提取后测定稀土元素的形态特征。结果表明,矿区果园表层土壤中稀土元素总量高于非矿区土壤的稀土元素含量,也高于我国土壤稀土元素含量的平均值,且矿区果园土壤的稀土属典型的富含重稀土元素的离子吸附矿型;矿区果园土壤中可氧化态和可还原态稀土元素含量占总含量百分比分别为61.6% 和31.9%,而酸溶态和残渣态稀土元素含量占总含量百分比则仅为4.4% 和1.98%,表明矿区果园土壤中稀土元素相对稳定,生物活性不高。实验测得矿区果园产的脐橙果肉中稀土元素含量为0.215mg/kg,远低于2005 年颁布的食品污染物限量标准(GB 2762 - 2005)中规定的水果类稀土氧化物限量值(≤ 0.7mg/kg),表明矿区果园脐橙中稀土元素含量对人体无害。     

脐橙凝胶型果派产品配方优化及工艺研究

以新鲜脐橙果浆、食品亲水胶体、果葡糖浆与白砂糖为主要原料制备脐橙凝胶型果派产品。以感官品评总体评价分值为产品质量评价指标,在单因素实验结果基础上,通过正交实验获得最优配方为:47.0%(质量比)甜味剂(果葡糖浆:白砂糖为1.3∶1)、13.0%(质量比)脐橙果浆、1.7%(质量比)胶凝剂(琼脂1.3%、黄芪胶0.2%、卡拉胶0.2%)、1.1%(质量比)柠檬酸。该配方下制备的产品色泽均一,具典型脐橙香味,酸甜味适中,并具良好的咀嚼性和弹性等质构特性。     

雪莲、脐橙复合果汁的护色及感官评价

在雪莲果、脐橙复合果汁中,脐橙可抑制多酚氧化酶的活性,具有护色作用。分别研究了脐橙、抗坏血酸(VC)和柠檬酸对复合果汁的护色效果,并通过正交实验确定了脐橙与复合护色剂的最优组合;用模糊数学法对复合果汁进行感官评价。结果表明:复合护色剂与脐橙的联合护色效果较好,其最佳配比是0.02% VC,0.3%柠檬酸,15%脐橙,此时复合果汁中残余PPO相对酶活为0.19%。模糊数学法对复合果汁的感官综合评价结果为"优",表明该果汁的感官性能很好,易于被消费者认可。     

基于可见/近红外光谱和变量选择的脐橙可溶性固形物含量在线检测

为联合可见/近红外光谱技术和变量选择方法在线检测脐橙主要内部品质指标可溶性固形物(SSC),分别选定脐橙校正集和预测集样本141个和47个,脐橙运输速度为0.3m/s,利用USB4000微型光谱仪在线采集脐橙样本的可见/近红外光谱,先分别采用无信息变量消除(UVE)和遗传算法(GA)对650~950nm波段范围的波长变量进行预筛选,再分别利用竞争自适应重加权采样(CARS)及连续投影算法(SPA)对波长变量进一步筛选,并应用偏最小二乘(PLS)方法分别建立脐橙SSC的在线预测模型,并与原始光谱等建立的预测模型进行比较。结果表明,对于脐橙SSC,预筛选方法GA优于UVE方法,变量选择方法CARS优于SPA方法;GA-CARS及GA-SPA联合变量选择方法优于对应的单一变量选择方法CARS及SPA。在上述变量选择方法中,GA-CARS方法获得的结果最优,其所建立的脐橙SSC的PLS模型的校正集和预测集相关系数分别为0.933和0.824,校正集和预测集均方根误差分别为0.429%和0.670%,性能优于原始光谱建立的PLS模型,且建模波长变量数由1 385个下降为78个,仅占原波长变量数的5.63%。由此表明,GA-CARS联合变量选择方法可以有效筛选脐橙SSC的波长变量,提高预测模型的稳定性和预测精度。     

微波消解-火焰原子吸收法测定花生中的铜、锌和铁

试验采用微波消解系统消解花生样品,将研碎的样品置于密闭容器内,加入一定量的硝酸和双氧水,放在微波炉中进行消解。采用正交试验设计确定微波消解花生的最佳工作参数。用火焰原子吸收法测定花生中铜、锌、铁的含量,其相对标准偏差(n=8)分别为0.99%、0.96%、1.89%,平均加标回收率分别为100.25%、99.44%、99.95%。该方法省时省酸,减少环境污染,准确度和精密度均优于传统方法。     

四个品种赣南脐橙果皮精油提取及挥发性成分分析

以四个品种赣南脐橙(纽荷尔、朋娜、华盛顿、奈维林娜)为原料,通过检测其可溶性糖、可滴定酸、可溶性固形物含量与固酸比,确定了四个品种果实的成熟度,并利用水蒸气蒸馏法提取果皮精油,采用气相色谱-质谱联用仪对挥发性成分进行研究,比较四个品种在精油得率和挥发性成分及相对含量上的差异。结果表明:四个品种脐橙的固酸比均大于或等于20.0,均已达到成熟状态;各脐橙果皮精油得率为:纽荷尔(1.05%)＞奈维林娜(0.94%)＞华盛顿(0.91%)＞朋娜(0.75%);样品中共鉴定出21种挥发性成分,包括13种烯烃类、3种醇类和5种醛类,烯烃类化合物是其主要挥发性成分。其中,纽荷尔脐橙果皮中鉴定出11种,d-柠檬烯(92.962%)、月桂烯(2.851%)和罗勒烯(1.039%)为其主要香气成分;朋娜脐橙果皮中鉴定出13种,d-柠檬烯(92.328%)、月桂烯(2.700%)和3-亚甲基-6-(1-甲基乙基)环己烯(1.020%)为其主要香气成分;华盛顿脐橙果皮中鉴定出14种,d-柠檬烯(92.322%)和β-蒎烯(2.653%)为其主要香气成分;奈维林娜脐橙果皮中鉴定出11种,月桂烯(47.036%)、2-蒎烯(15.313%)、3-亚甲基-6-(1-甲基乙基)环己烯(11.593%)为其主要香气成分。本研究结果为赣南脐橙品种精油的开发利用提供参考。     

微波消解-氢化物原子吸收光谱法测定豆豉中铅的含量

建立了用微波消解样品、氢化物原子吸收光谱法测定豆豉中重金属铅的方法。研究了消解试剂、消解温度和消解时间对样品消解效果的影响,优化了氢化物原子吸收光谱法测定铅的条件。在选定的实验条件下,铅的线性方程为:C=73.15A-0.958,r=0.998,表明铅溶液在0～20μg/L范围内呈良好的线性关系。方法检出限为0.08μg/L(S/N=3)。加标平均回收率为93.4%～95.8%,相对标准偏差为4.50%～6.25%(n=6)。该方法灵敏度高、操作简单,在实际测定中取得满意结果。     

Effect of Gastric Digestion pH on Iron, Zinc, and Calcium Dialyzability from Preterm and Term Starting Infant Formulas

ABSTRACT: Iron, zinc, and calcium dialyzability from preterm and term starting infant formulas were determined after in vitro digestion, using special gastric conditions prevailing in preterm and newborn infants. Mineral dialyzability was studied using pH 2.0,3.5, and 4.5 for gastric digestion. The effect of gastric pH was more important on iron dialyzability (FeD) and zinc dialyzability (ZnD) than on calcium dialyzability (CaD). The effect on iron dialyzability was remarkable in fluid formulations with high digestibility: FeD was 18% to 20% when gastric digestion was made at pH 2, decreasing to 3% when made at pH 4.5. In most powder infant formulas with the lowest digestibility, FeD remained close to 10% despite variations in gastric digestion pH. Percent zinc dialyzability (ZnD%) steadily decreased when gastric digestion pH increased. At each pH, percent iron dialyzability (FeD%) and ZnD% from human milk were higher than those from infant formulas. Evaluation of mineral dialyzability from these infant formulas, using a gastric digestion pH prevailing in preterm and newborn infants, can provide valuable information on mineral availability.     

Determination of Ca,Cd, Cu,Fe, K,Mg, Mn,Mo, Na,Se, and Zn in Foodstuffs by Atomic Spectrometry After Sample Preparation Using a Low-Cost Closed-Vessel Conductively Heated Digestion System

Establishing fast, simple, low-cost, and efficient sample preparation procedures to determine elements in foodstuffs is a relevant aspect for nutritional and health purposes. For this reason, the recently proposed closed-vessel conductively heated digestion system (CHDS) was evaluated for the digestion of milk powder, chocolate powder, and soluble coffee samples aiming for Ca, Cu, Fe, K, Mg, Mn, Na, and Zn determinations by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and Cd, Mo, and Se determinations by inductively coupled plasma mass spectrometry with tandem configuration (ICP-MS/MS). The accuracy was evaluated by analyzing two milk certified reference materials digested by the CHDS and a microwave oven for comparison. When using the CHDS, recoveries for the analytes varied from 91 to 104 %. For microwave digestions, recoveries within the 94–109 % intervals were obtained. The method was then applied to the samples. For comparative purposes, the analytes were also determined in the samples after microwave digestion, and the results between the two digestion systems showed no differences based on a paired t test at a 95 % confidence level. Similar analytical blanks were obtained because quartz digestion tubes were used in both digestion systems. The CHDS with quartz tubes is an interesting alternative for laboratories dedicated to large-scale routine analysis because volatile elements usually found in very low concentrations in food samples such as Cd and Se can also be determined.     

Feed intake and digestion by Holstein steers fed warm or cool season grass hays with corn, dried molasses, or wheat middlings.

This study determined the effects of adding a small amount of dried molasses to supplemental corn and of supplementing with corn, wheat middlings, or corn-wheat middlings mixture on intake and digestion by Holstein steers fed warn or cool season grass hays. Eight steers (175 kg BW), in two simultaneous Latin squares, were fed, once daily, bermuda-grass (72% NDF) or ryegrass-wheat (58% NDF) hay ad libitum, alone or with approximately .05% BW of dried molasses (with 31% roughage), 5% BW of ground corn, or both. Adding dried molasses to corn decreased feed intake but did not affect digestible OM intake. Total tract digestion of fiber from bermudagrass tended to be enhanced by adding dried molasses to corn. Eight steers (193 kg BW) were used in an experiment with the same design in which similar forages were fed alone or with corn (.5% BW), wheat middlings (.63% BW), or .25% BW of corn plus .31% BW of middlings. Feed intake for both grasses was similar among supplements. Wheat middlings depressed total tract fiber digestion more than corn with both forages. Supplementation with corn depressed fiber digestion slightly more with ryegrass-wheat than with bermudagrass, but wheat middlings had a slightly greater depressing effect on fiber digestion with bermudagrass. Associative effects of mixing corn and wheat middlings in OM digestion and digestible OM intake were negative for bermudagrass and positive for ryegrass-wheat. Interaction among characteristics of basal forage and concentrate modulated feed intake and digestion by ruminants.     

Dietary sodium bicarbonate and magnesium oxide for early postpartum lactating dairy cows: effects on production, acid-base metabolism, and digestion

In two experiments with cows in early lactation fed 40% corn silage and 60% concentrate diets (dry basis), we examined effects of 1.0% dietary sodium bicarbonate and .8% magnesium oxide in a 2 x 2 factorial arrangement on performance, acid-base metabolism, and digestion. In Experiment 1 with 20 Holstein and 4 Jersey cows, intake and milk production were not affected by treatment through 12 wk postpartum. In digestion trials at 3, 6, 9, and 12 wk postpartum, addition of magnesium oxide increased digestibility of dry matter 1.8% units by sodium bicarbonate whereas acid detergent fiber digestion increased 9 to 12% units with addition of either buffer. In Experiment 2, with four fistulated Holstein cows in a Latin square design, intake per unit body weight was increased .18% units by dietary sodium bicarbonate while milk production was unaffected. Dry matter and acid detergent fiber digestion were increased slightly by sodium bicarbonate plus magnesium oxide addition whereas nitrogen balance increased 23 g/day in cows fed magnesium oxide alone. Because of the low fiber content of the ration, milk fat percent increased .5 to .9% by addition of either buffer in both experiments and resulted in corresponding increased in fat-corrected milk. Sodium bicarbonate and magnesium oxide prevented rapid declines in rumen pH associated with feeding in Experiment 2, which related to changes in acid detergent fiber digestion. Blood acid-base metabolites were relatively unchanged by treatment in either experiment. Urinary bicarbonate and net acid excretion rates were changed on the average by +41 and +43 meq/h by sodium bicarbonate or magnesium oxide but could not be related to changes in intake and production.     

Effects of feeding milk replacer at 2 rates with pelleted,low-starch or texturized,high-starch starters on calf performance and digestion

Milk replacer (MR) feeding programs have traditionally fed at less than ad libitum amounts to promote calf starter (CS) intake and allow early weaning. More recently, increased amounts of MR preweaning have been shown to increase preweaning ADG, although postweaning growth may be reduced. Several studies suggest that limited postweaning digestion of nutrients in CS may contribute to postweaning growth impairment. It is not clear whether CS formulation might also contribute to differences in postweaning nutrient digestion when calves are fed different MR programs. A 56-d feeding and digestion trial was conducted to compare growth and digestion in 2- to 3-d-old male Holstein calves (n = 48; initially 41.9 kg of body weight) fed a moderate (MRM) or high (MRH) MR program and either a pelleted CS containing 9.9% starch or a texturized CS containing 41.3% starch. Programs were 0.66 kg of dry matter (DM)/d of MR to d 46, then 0.33 kg/d to d 49 (MRM) and 0.85 kg of DM/d to d 5, then 1.07 kg/d to d 42, then 0.53 kg/d to d 49 (MRH). The MR contained 25% crude protein and 18.6% fat and was reconstituted to 13 (MRM) or 15% (MRH) solids. Calves were also assigned randomly to receive a pelleted CS (9.9% starch, 36.9% NDF) or a textured CS (41.3% starch, 13.3% NDF) and water for ad libitum intake for 56 d. During d 31 to 35 and 52 to 56, fecal samples were collected from 5 calves per treatment for estimates of digestibility. Selected nutrients and chromic oxide (d 31–35) or acid-insoluble ash (d 52–56) were analyzed in feed and feces to estimate digestibility. Data were analyzed as a completely randomized design. Repeated measures analysis was performed when data were measured by week. Calves fed MRH gained more body weight (but not hip width) and were more efficient to weaning compared with calves fed MRM, although fecal scores and days treated with medications were greater. We found no effect of CS on animal performance, although calves fed textured CS had higher fecal scores. Digestibilities of nutrients were affected by treatment and time of sampling (5 or 8 wk). At 5 wk, digestion of DM, organic matter, crude protein, and fat were lower and digestion of acid detergent fiber, neutral detergent fiber, and starch were higher in calves fed MRM and reflected greater CS intake. Also, digestion of DM, organic matter, acid detergent fiber, starch, crude protein, and fat were greater in calves fed textured CS at 5 wk. By 8 wk, when CS was the only source of nutrients, digestion of DM, organic matter, acid detergent fiber, and neutral detergent fiber were greater in calves fed MRM and digestion of DM and organic matter were greater, and acid detergent fiber and neutral detergent fiber digestion were lower in calves fed textured CS. Formulation of CS as well as amount of MR offered to young calves influenced animal performance and digestion in this study.     

Effects of niacin and whole cottonseed on ruminal fermentation, protein degradability, and nutrient digestibility

Four mature nonlactating Holstein heifers fitted with ruminal and duodenal cannulae were used to investigate in vivo effects of niacin and whole cottonseed. Each heifer was assigned randomly to a treatment in a 2 X 2 factorial arrangement of treatment sequences within a 4 X 4 Latin square design. Heifers were fed isonitrogenous complete mixed rations individually twice daily. Diets contained corn-soybean meal concentrate, corn silage, chopped coastal bermudagrass hay, plus 1) 0% niacin and 0% whole cottonseed, 2) 0% niacin and 15% whole cottonseed, 3) .07% niacin and 0% whole cottonseed, or 4) .07% niacin and 15% whole cottonseed. Dry matter consumption, ruminal pH, ruminal ammonia and VFA concentrations, microbial N production, and DM and ADF digestion were not affected by treatment. Numbers of ruminal protozoa and RNA concentrations were reduced with whole cottonseed feeding and increased by addition of niacin. Whole cottonseed increased molar percentages of acetate while depressing propionate. Niacin supplementation resulted in greater digestion of both CP and NDF. Ether extract digestibility was highest in heifers fed whole cottonseed. Fiber digestion was not affected by whole cottonseed feeding.     

电感耦合等离子体发射光谱法测定鲜榨西瓜汁中铁钙镁钾钠磷

用硝酸和过氧化氢的混合消解液对鲜榨西瓜汁进行封闭微波消解,采用电感耦合等离子体发射光谱仪（ICP-AES）法直接测定西瓜汁中微量铁、钙、镁、钾、钠、磷的含量。该方法检出限符合规范要求,方法回收率98.5%～101.8%,相对标准偏差（RSD）〈5.0%。该方法具有良好的准确度和精密度,且溶样过程无污染,方法简便、快速。     

Ruminal degradation of dried brewers grains, wet brewers grains, and soybean meal

A series of trials was conducted to determine the ruminal degradation of nitrogenous compounds and dry matter of soybean meal, wet brewers grains, and dried brewers grains. In situ and in vitro estimates of degradation were positively correlated but yielded different absolute values for measures of ruminal degradation. Ruminal digestion of protein, predicted from in situ data, was 42, 73, and 83% for brewers dried grains, brewers wet grains, and soybean meal. Drying of wet grains at either 50 or 150 degrees C increased resistance to ruminal digestion equally. Measurements of flow of dry matter and nitrogen of feed origin to the duodenum were made in vivo for diets containing either brewers dried grains or soybean meal. Negative apparent digestibility of nitrogen in the rumen for a 13% crude protein, brewers dried grains ration indicates the potential for using a non-protein nitrogen supplement with this ration. Resistance to digestion of nitrogen from brewers dried grains occurred only in the rumen. Amino acid patterns delivered to the small intestine and digestion of duodenal contents were similar for diets containing brewers dried grains or soybean meal.     

Changes in the forms of iron and in concentrations of taurine, carnosine, coenzyme Q(10), and creatine in beef longissimus muscle with cooking and simulated stomach and duodenal digestion

Longissimus muscle samples from 31 Angus-cross heifers finished on either a high-concentrate feedlot diet or pasture were used to evaluate the effects of cooking (71°C) on the concentration and forms of iron in the meat, and also on concentrations of the bioactive compounds taurine, carnosine, coenzyme Q(10), creatine and creatinine. For a sub-sample of 15 the effects of pepsin and pancreatin digestion were assessed. For iron, cooking resulted in some overall loss together with a major change from soluble haem and non-haem iron to the insoluble forms, but solubility was regained to a significant extent following digestion. Total haem iron percentage, however, decreased at each step from an initial 88% to a final 61% of total iron. For the bioactive compounds, cooking led to a reduction in taurine, carnosine, coenzyme Q(10), and creatine. The effects of digestion on the bioactive compounds varied. No clear differences were shown in the way in which beef from pasture-finished and feedlot-finished cattle responded to cooking and digestion.     

石墨消解-微波消解法测定乳粉中总砷、总汞、铅和镉

目的建立石墨消解-微波消解法测定乳粉中的总砷、总汞、铅和镉含量的分析方法。方法样品经石墨加热预消解,采用微波消解法前处理,并采用电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定乳粉中的总砷、总汞、铅和镉含量。结果总砷、总汞、铅和镉的平均加标回收率为94.4%?108.3%,精密度的相对标准差(relative standard deviation,RSD)为1.1%?4.6%,方法检出限分别为4.4、4.8、4.9、0.6?g/kg。乳粉质控样和考核样中总砷、总汞、铅和镉的测定结果均在参考值范围内,结果均为满意。结论该方法操作简便,重现性良好,测定结果准确、可靠,适用于乳粉中总砷、总汞、铅和镉的含量测定。