Solid fat content determination using ultrasonic velocity measurements

The ultrasonic group velocity has been measured through 0–20% mass fraction samples of tristearin, tripalmitin, trilaurin and 1-oleodipalmitin suspended in paraffin oil at 25°C and 1 MHz. For tristearin, tripalmitin and trilaurin there is an increase of about 3.1 m/sec per 1% increase in insoluble triglyceride in suspension. For trilaurin and 1-oleodipalmitin there is a slight decrease in velocity with increasing soluble triglyceride. The technique may, therefore, prove useful for determination of solubilities of triglycerides in suspension, as well as for determining solid fat contents. For the tristearin/paraffin oil suspensions there is a good correlation between the solid content added and that predicted by a theoretical formula available in the literature (correlation = 0.998 for twenty samples). The reproducibility of the solid fat content determination is 0.2%, the accuracy is about 0.6%. The technique is easily automated, cheap, accurate, rapid and non-intrusive and should, therefore, prove useful both as an in-line quality control monitoring device and as a new instrumental technique for research applications.     

Ultrasound Doppler based in‐line viscosity and solid fat profile measurement of fat blends

This study reports the use of upgraded ultrasonic velocity profiling with pressure difference methodology; extended from previous work demonstrating true in‐line rheological and solid fat content (SFC) characterisation of complex opaque fat blends, subjected to scaled dynamic processing conditions. The experimental results have successfully confirmed previous non‐invasive, in‐line measurements for instantaneous velocity and rheological profiling of complex opaque fat blends [International Journal of Food Science and Technology 43 (2008) 2083]. A method for in‐line measurements under dynamic processing conditions to obtain the SFC of a fat blend was developed and successfully tested for a 30% palm stearin and 70% rapeseed oil system over a temperature range of 10–40 °C. These measurements correlated well with standard SFC values from pulsed‐nuclear magnetic resonance (p‐NMR) measurements deviating not more than +/– 2% SFC points from the standard p‐NMR values.     

In Situ Ultrasonic Characterization of Cocoa Butter Using a Chirp

Differences between tempered and untempered cocoa butter were investigated by an ultrasonic signal “chirp” generated by contact transducers. Polarized light microscopy and powder X-ray diffraction were used to characterize the morphology and polymorphism of tempered and untempered cocoa butter, whereas pulsed nuclear magnetic resonance was used to determine the amount of crystalline solids present. Ultrasonic wave velocity and attenuation data were collected simultaneously throughout the 5-h crystallization process for cocoa butter. Ultrasonic velocity and attenuation changed at the different solid fat contents (SFC): 4, 8, and 11 %. Untempered cocoa butter showed an attenuation of 3 dB/cm at 1.7 MHz and 4 % SFC, whereas tempered cocoa butter showed an attenuation of 4.5 dB/cm at 1.7 MHz and 4 % SFC. At 3 MHz, the attenuation was 2 dB/cm for untempered and 6 dB/cm for tempered cocoa butter. Under these conditions (4 % SFC, 3 MHz), the chirp wave of tempered sample showed a phase angle change of 0.5 rad, whereas the untempered sample showed ?0.5 rad relative to the canola oil that was taken as 0. The study suggests that an ultrasonic chirp can be effectively used to detect differences between tempered and untempered cocoa butter when measuring attenuation and ultrasonic wave phase angle changes as a function of frequency. The in-line characterization of chocolate “temper” using such nondestructive ultrasonic measurements could be applied to industrial chocolate manufacturing.     

Rapid Determination of Total and Solid Fat Contents in Chocolate Products by Pulsed Nuclear Magnetic Resonance

A rapid pulsed NMR method of fat analysis in chocolate without prior solvent extraction was developed. Total fat content of 43 chocolate products was determined at 60°C using sucrose-oil mixtures as standards. Solid fat content (SFC) was calculated from the liquid oil content at different temperatures. Total fat content agreed to 0.90% standard error of prediction as compared with the Soxhlet method. SFC as determined by NMR correlated well with the dilatometry (r = 0.98) and the DSC (r = 0.96) results. This technique is suitable for quality control of chocolate and other lowmoisture, high-fat products.     

Measurement of solid fat content by ultrasonic reflectance in model systems and chocolate

A series of confectionery coating fat (CCF) and cocoa butter (CB) dispersions in corn oil were prepared and tempered to a range of temperatures (10, 12 and 15 °C and 26, 27.5 and 29 °C respectively) to produce samples with solid fat contents (SFC) between 0 and 9%. The ultrasonic velocity in the CCF samples increased with increasing SFC and decreased with temperature, however the CB samples were too attenuating to allow velocity measurements. The ultrasonic reflectance at the surface of both sets of dispersions decreased linearly with SFC but at the same level of solids was less for CB than CCF suggesting some dependence on other aspects of fat structure. The microstructures and thermal properties of the fat systems are compared in an attempt to understand these structural differences. Finally ultrasonic reflectance is shown to respond to changes in a chocolate melt during tempering.     

月见草油微胶囊粉末油脂中油脂过氧化值测定之提油方法的研究

为测定月见草油微胶囊粉末油脂中油脂过氧化值,比较了碱性乙醚法、机械研磨法、超声波振荡法提油的优劣,结果表明:碱性乙醚法提油率虽高(94.69%),但测得的POV值与原料油相比偏高很多,明显失真;机械研磨法提油率偏低(40.68%),且不稳定,不宜采用;超声波振荡法提油率居中(59.63%),重现性好,精确度高,POV测定值与原料油最接近;试验还表明超声振荡时间以3min为宜。     

基于水蒸气蒸馏法的狮头柑精油提取工艺优化及成分分析

为优化狮头柑精油的水蒸气蒸馏提取工艺,以狮头柑果皮鲜样为材料,采用超声辅助处理,在优选蒸馏设备和单因素实验基础上,对超声温度、超声功率及超声时间3因素进行响应面优化研究,并采用气相色谱-质谱法（GC-MS）对所得精油进行成分分析。结果表明:采用Clevenger挥发油蒸馏仪的提取效果优于其他3种蒸馏设备;响应面分析得到狮头柑精油最优提取工艺为:超声温度33 ℃、超声功率80 W、超声时间32 min,此条件下精油得率可达到2.50%±0.02%。从狮头柑精油中共鉴定出29种化合物,占总挥发物的99.16%,包括烯烃类（主要为D-柠檬烯,含量可达88.35%）、醇类（主要为芳樟醇0.18%）、醛类（主要为正辛醛0.17%）等。该研究技术可用于狮头柑果皮精油的提取。     

Influence of SFC, microstructure and polymorphism on texture (hardness) of binary blends of fats involved in the preparation of industrial shortenings

Several binary blends of vegetable oils commonly used in industrial shortenings (i.e., palm oil (PO), hydrogenated palm oil (HPO), soybean oil (SO), hydrogenated soybean oil (HSO), low-erucic acid rapeseed oil (LERO), hydrogenated low-erucic acid rapeseed oil (HLERO)) were studied for their physical properties such as solid fat content (SFC) by nuclear magnetic resonance (NMR) and textural properties (hardness). Microstructure was also observed by microscopy in order to explain the variability in hardness for samples having the same SFC values. The blends studied by microscopy were the following: HSO, HPO and HLERO diluted in LERO. For these three blends which had the same SFC, the level of network structure was different. HSO diluted in LERO had more crystals, closer to each other and overlapped. This can explain that HSO has a higher hardness than HPO or HLERO, for a same SFC value, when diluted in LERO. Polymorphism was also observed by powder X-ray diffraction. The variability in hardness for samples having the same SFC is due to various crystal types and/or network structures that are formed upon crystallization of hard fats. This work demonstrates that for binary blends of studied oils, changes in the hardness are controlled mostly by the SFC, polymorphism and also by the material’s microstructure.     

The advantages of solid fat content determination in cocoa butter and cocoa butter equivalents by the Karlshamns method

This paper describes the preparation of samples and the evaluation techniques applied to determine the Solid Fat Content (SFC) by means of pulsed nuclear magnetic resonance (NMR) in confectionery fats characterized by distinct polymorphism (cocoa butter, cocoa butter equivalents and their mixtures). Due to the deviation of SFC values in certain softer cocoa butter equivalents at the temperature of 20 °C, an internal method devised at Karlshamns Oils & Fats AB is applied as well. When compared to the official IUPAC 2.150 (b) method, Karlshamns' method involves a lower temperature and a prolonged period of time at the stage of the final SFC stabilization in the pre-treatment of fat samples. The calculation of SFC in the analysed samples for the purposes of this paper was carried out by employing both methods (the indirect method and a serial procedure). The results are presented graphically. Differences were reflected in the SFC of the fats and their mixtures that were under observation depending on the method and temperatures applied. The obtained results indicated a considerable advantage of employing the Karlshamns method since the results yielded by this method are more lucid. Moreover, the behaviour of fats in the production process can be more easily predicted on the basis of these results.     

Production of zero trans Iranian vanaspati using chemical transesterification and blending techniques from palm olein, rapeseed and sunflower oils

Chemical transesterification and blending techniques were used for producing zero trans fats suitable for use as Iranian vanaspati. Triple blends of palm olein (POo), rapeseed (RSO) and sunflower oil (SFO) were subjected to two different treatments: (i) blending and then transesterification (BT) and (ii) transesterification of pure POo before blending with RSO and SFO (TB). The changes in slip melting point (SMP), solid fat content (SFC), carbon number (CN) triacylglycerol (TAG) composition, induction period (IP) of oxidation at 120 °C and IP of crystallisation at 20 °C of blends before and after treatments were investigated. Both BT and TB methods resulted in an increase in the CN48 TAG molecules, SMP and SFC, and a decrease in the IP of oxidation and crystallisation of initial blends. Samples made by TB method had higher CN48 TAG content, SMP, SFC and IP of oxidation, and lower IP of crystallisation than those made by BT method. Correlation between SFC at 20 °C and saturated fatty acid (SFA) content of the treated blends indicated that the SFA must be higher than 33.1% and 26.8% for BT and TB methods, respectively, to obtain fats suitable for use as vanaspati.     

超声改性大豆分离蛋白与大豆可溶性多糖复合乳化体系的冻融稳定性研究

本实验针对不同超声功率改性的大豆分离蛋白与大豆可溶性多糖形成的复合乳液的冻融稳定性进行研究, 揭示乳液冻融稳定机理与形成乳液复合物结构特性之间的构效关系。对2 次冻融循环处理前后乳液油滴进行共聚焦 观察,研究等温结晶固脂含量、油脂被乳化量的变化和作为乳化剂的大豆分离蛋白不同超声处理（0、200、300、 400、500 W）下二级结构的变化,进而分析其与乳液冻融稳定性的关系。结果表明：乳液经2 次冻融循环处理后 随着超声功率的增加聚结程度降低,400 W超声处理的大豆分离蛋白与大豆可溶性多糖复合乳液最为稳定;等温 结晶条件下不同乳液固脂含量增加速率不同,但最终平衡时总含量相同;油脂被乳化量发生不同程度的变化;不 同超声处理改变了大豆分离蛋白的二级结构,400 W超声处理的大豆分离蛋白无规卷曲结构含量最高。说明不同 超声改性的大豆分离蛋白与大豆可溶性多糖会形成不同结构的复合物,影响了乳液的冻融稳定性,初步明确了 适当的超声处理能够改善大豆分离蛋白的空间结构,促进其与大豆可溶性多糖分子的键合,进而影响大豆分离蛋 白-多糖界面结构特性和乳化体系的冻融稳定性。     

Monitoring Tempered Dark Chocolate Using Ultrasonic Spectrometry

Ultrasonic spectrometry was used to distinguish between properly tempered and untempered commercial dark chocolate. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) were used to characterize the polymorphic state of tempered and untempered chocolate, results that were correlated to those of ultrasonic spectrometry. Four different kinds of dark chocolate samples with different amounts of sugar (7.5–50 %), fat (30–50 %), and cocoa mass (70–90 %) were subjected to two different tempering protocols. The tempering was achieved using cocoa butter seeds under static cooling from 50 to 14 °C. The ultrasonic generator and analyzer SIA-7 (V.N. Instruments) was used to monitor the crystallization process. The instrument generated a chirp signal with a bandwidth of 0.5 to 3 MHz and was set to work in a four-pathway configuration with two transducers and a center frequency of 2.25 MHz. Spectrometric analysis was carried out with chocolate samples containing 2, 4, and 6 % solid fat content (SFC). The SFC was obtained from DSC measurements. Ultrasonic signals for attenuation, reflection, and velocity were compared between tempered and untempered chocolates. It was shown that seed-tempered chocolate with 30 % sugar and 47.5 % fat attenuated 2.5 MHz of ultrasonic waves by 0.8, 1.7, and 2.0 dB/cm at 2, 4, and 6 % SFC, respectively. On the other hand, untempered chocolate attenuated the ultrasound signal by 3.5, 3.6, and 4.3 dB/cm. Furthermore, it was found that ultrasound reflection signals were stronger and ultrasonic velocity was higher in chocolates with high sugar content.     

COMPARISON OF LINOLEIC AND CONJUGATED LINOLEIC ACIDS IN ENZYMATIC ACIDOLYSIS OF TRISTEARIN

The acyl incorporation and migration of linoleic and conjugated linoleic acids in enzymatic acidolysis were compared in a solvent-free system. Two systems were used in the Lipozyme RM IM-catalyzed acidolysis at 60C temperature and 5% by weight enzyme load (based on substrates). One included tristearin (SSS) and linoleic (L) or conjugated linoleic (cL) acids (1:6, mol/mol). The other was between tristearin and the mixture of linoleic and conjugated linoleic acids (1:3:3, mol/mol/mol). Acyl incorporation and migration together with triacylglycerol composition of the products were monitored with gas chromatography, pancreatic lipase hydrolysis, and high performance liquid chromatography. Both acyl incorporation and migration of linoleic acid were faster than those of conjugated linoleic acid. At 5 h reaction, there were 13.0% LLL, 46.5% LSL, 27.7% LSS, and 5.6% SSS in the product for a system between tristearin and linoleic acid; whereas there were 2.4% cLcLcL, 10.4% cLScL, 50.9% cLSS, and 36.2% SSS in the product for a system between tristearin and conjugated linoleic acid. The results suggest that linoleic acid was more reactive than conjugated linoleic acid in the enzymatic acidolysis probably because of the rigid structure of the latter.     

Monitoring the Polymorphic Transformation of a Palm Kernel-Based Emulsion Using Ultrasound

Ultrasonic spectrometry was used to monitor the changes in polymorphism of palm kernel fat present in two tempered non-dairy emulsions with different globule sizes. Laser diffraction and differential scanning calorimetry (DSC) were performed to characterize the emulsions. X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) were used to determine the polymorphic state and solid fat content (SFC) of fully hydrogenated palm kernel oil during tempering of the emulsions. The ultrasonic instrument generated a “chirp” signal, which is characterized by its bandwidth. The ultrasonic measurements were carried out using two different pairs of transducers with different center frequencies, 2.25 and 0.5 MHz, and bandwidths. 3D plots were generated disputing time, frequency, and signal strength. The whole tempering process, from start to finish, was better characterized with the 2.25-MHz center frequency transducers. The ultrasonic velocity through the emulsions was always higher for the more stable β′ polymorph than for the α polymorph (p?<?0.05) regardless of the pair of transducers used. The 2.25-MHz transducer revealed no significant difference (p?>?0.05) on the ultrasound velocities obtained for the two globule sizes. Monitoring of polymorphic changes in emulsions using ultrasonic spectrometry could be used for an online measurement system for industrial manufacturing.     

基于低共熔溶剂法超声辅助蒸馏提取胡椒叶精油的工艺优化及其GC-MS分析

以胡椒叶为提取原料,探究低共熔溶剂对胡椒叶精油提取效果的影响。在单因素实验结果的基础上,以液料比、超声功率与蒸馏时间为影响因素,以精油得率为响应值,应用Box-Behnken试验设计建立数学模型,进行响应面分析。结果表明,氯化胆碱-尿素组成的低共熔溶剂提取效果最好,响应面优化的最佳提取工艺条件为液料比为14:1 mL/g、超声功率300 W、蒸馏时间53 min。在此条件下,胡椒叶精油得率为1.380%±0.018%,优于水蒸气蒸馏法和超声辅助水蒸气蒸馏法,胡椒叶精油得率分别提升了14.33%、5.18%。通过GC-MS对胡椒叶精油进行分析,共鉴定出34种化合物,其主要成分为δ-榄香烯(19.75%)、α-荜澄茄油烯(9.17%)、石竹烯(8.97%)、α-古芸烯(6.12%)、β-榄香烯(5.13%)。结果表明,以氯化胆碱-尿素作为低共熔溶剂提取胡椒叶精油的方法是可行的。     

反胶束萃取大豆油脂及其与浸出法的比较研究

采用超声辅助2种反胶束体系萃取大豆油脂,分析超声波技术影响反胶束萃取大豆油脂的主要因素,并分析所得油脂的品质与之浸出法进行了对比.经试验研究得到,最佳的工艺条件为超声时间lh、超声温度60℃、超声功率300 W、全脂豆粉加入量为0.04 g/mL;2种不同反胶束体系萃取大豆油脂的萃取率差别不大,AOT反胶束法的前萃率为81.39％,AOT-Tween85反胶束法的前萃率为84.17％.反胶束萃取得到的油脂,酸价及过氧化值比浸出法要低;浸出法、AOT反胶束法、AOT-Tween85反胶束法3种方法提取的大豆油脂脂肪酸组成和含量基本相同,色泽、皂化值也基本相同,碘值稍有差异.     

Influence of Surface Structure on Cholesterol Oxidation in Model Food Powders

Three milk-resembling powders having different oil phases were prepared and stored for six months at room temperature. Samples were taken monthly for estimation of the surface composition by ‘electron spectroscopy for chemical analysis’ (ESCA) and analyses of the level of cholesterol oxides by gas chromatography. The highest fat coverage was obtained with technical tristearin as the oil phase. This preparation had around 75% of the powder surface covered by fat; during storage this coverage decreased. This powder also had the largest increase in cholesterol oxides during storage, the final level being 159 μg g⁻¹ cholesterol. The powder containing high-melting pure tristearin had a low surface coverage of fat, originally about 25%, which decreased during the storage period. Little increase in cholesterol oxides was observed, the final level being 52 μg g⁻¹ cholesterol. The third powder containing liquid triolein as oil phase, had a surface coverage of about 50% throughout the storage period. The cholesterol oxidation rate was in between that of the two tristearin powders, the final level of oxides being 75 μg g⁻¹ cholesterol. The results for the investigated powders indicate that the surface composition is of major importance for the oxidation of cholesterol. No correlation between cholesterol oxidation and solvent extractable fat (free fat) was found.     

超声波法制备八角茴香油-β-环糊精微胶囊及其表征分析

为提高八角茴香油的稳定性,采用超声波法制备八角茴香油-β-环糊精微胶囊。以包埋率为评价指标,通过正交试验优化制备工艺,并考察微胶囊的加热释放特性。结果表明,最佳制备工艺为八角茴香油与β-环糊精质量比1∶6(g/g)、超声时间40 min、超声温度50℃、超声功率198 W,在此条件下包埋率为94.21%,载药量为6.93%,平均粒径为2.53μm。超声温度和超声功率的变化对微胶囊包埋率的影响显著。红外光谱、差示扫描量热分析和热重分析证实了微胶囊的形成。释放特性表明,200℃条件下加热120 min,八角茴香油保留率仅剩4.60%,而相同温度和时间条件下,微胶囊中八角茴香油保留率为78.38%,是八角茴香油的17.04倍,八角茴香油被包埋后热稳定性提高。超声波法和饱和水溶液法制备微胶囊相比,载药量相差不大,但超声制备的微胶囊包埋率及收率比饱和水溶液法分别提高7.80%和4.98%;超声制备微胶囊包埋率、收率及载药量比研磨法分别提高14.68%、1.88%和1.85%。超声波法是制备高质量八角茴香油-β-环糊精微胶囊的简便可行方法,八角茴香油被包埋后稳定性提高,有望应用于食品保鲜领域。     

利用酯交换法改进棕榈油硬脂的加工性能

将棕榈油硬脂(ST)与大豆油(SBO)按不同比例混合再进行酯交换反应可以得到不同固脂特征的油脂。实验发现,其中的酯交换油脂IE(70%ST 30%SBO)最适合于加工成通用型起酥油。对这种酯交换油脂的打发性、软硬度及氧化稳定性进行了分析,并与目前市场上常见的全棕榈油基起酥油进行了比较,发现酯交换油脂的柔软度和打发性能均优于后者,但其氧化稳定性不及全棕榈油基起酥油。     

不同提取方法对红松籽油甾醇浸提及功能性质影响的研究

以有机溶剂浸提法为对照,研究超声波、微波、光波辅助溶剂法对红松籽油甾醇浸提效果及不同方法提取物的抗氧化、抑制胰脂肪酶活性和与胆酸盐结合能力。通过磷硫铁比色法测定甾醇得率,采用自由基清除体系、对硝基苯酚法、模拟体外消化实验法分别测定四种方法提取甾醇的自由基清除能力、脂肪酶活性抑制效果及胆酸盐结合能力。结果表明,微波辅助溶剂法（500 W,1 min）提取的红松籽油甾醇得率（2.263±0.013）mg/g最大（P<0.05）。四种提取方法中,微波辅助溶剂法提取的红松籽油甾醇对DPPH·清除效果最好,超声波辅助溶剂法提取的红松籽油甾醇对ABTS+·清除效果最好,超声波辅助溶剂法提取的红松籽油甾醇可显著抑制胰脂肪酶活性（P<0.05）,IC50值为（1.322±0.020）mg/mL,与牛磺胆酸钠、甘氨胆酸钠结合能力最强,分别为（77.593±1.401）%、（77.601±1.103）%。超声波辅助溶剂法提取的红松籽油甾醇得率略低于微波辅助溶剂法,但抗氧化能力、胰脂肪酶活性的抑制作用及胆酸盐结合能力均为最强,本研究为红松籽油甾醇的制备及功能性产品研发提供理论依据。