Effect of various irradiation doses on some nutrients of Pakistani date

Summary Date samples were irradiated with different doses using a gamma-irradiator. Levels of moisture, protein, fibre and fats were determined on monthly basis for 5 months. Generally, the moisture contents of control date samples packed in white polythene decreased from 14.1±1.1 to 9.7±0.8% over a 5-month period while the irradiated samples were in the range of 10.4-11.2%, however, no proper pattern of change was observed. After 5-month storage, the protein level of irradiated samples was reduced to 1.00-1.30%, while the percent fibre levels were found to be in the range of 2.40-2.48. Similarly, the fat level decreases from 1.06±0.12 to 0.68±0.06 for control date sample while after 5-month the decrease in fat content was 0.45±0.04%, 0.44±0.04%, 0.44±0.05%, 0.42±0.05% and 0.40±0.04% for samples irradiated with 20, 50, 100, 200 and 300 krads, respectively.     

应用近红外技术测定黄豆粕中水分、蛋白质和粗脂肪

应用近红外分析仪（NIR）快速测定黄豆粕中水分、蛋白质和粗脂肪的含量,通过光谱扫描统计分析,分别找出测量黄豆粕水分、蛋白质、粗脂肪的波长及校准常数值,经数理统计分析结果表明：近红外法与常规水分测定法经典凯氏定氮法、索氏浸提法所测定的结果呈密切的线性相关,检测结果令人满意。     

Comparison of two infrared spectroscopic methods for cheese analysis

Two infrared spectroscopic methods, optothermal near infrared (NIR) spectroscopy and Fourier transform mid-infrared-attenuated total reflection (FTIR-ATR) spectroscopy, were applied to 24 cheese samples in order to obtain protein, fat and moisture contents. Reference values of the protein, fat and moisture contents in weight percent were obtained using standard wet chemistry analysis. Prediction correlation coefficients between 0.93 and 0.96 and standard errors of prediction between 2% and 5% were obtained using optothermal spectroscopy while the corresponding values for FTIR-ATR were 0.81–0.92 and 4–9%. Inhomogeneities in the cheeses, primarily due to the fat droplets, are probably the main reason for the differences in the error sizes. The superior results for optothermal spectroscopy are the more attractive because the instrument is easier to use than the FTIR-ATR instrument, it provides results more quickly with simpler statistical analysis and it is more compact and robust.     

Determination of moisture, starch, protein, and fat in common beans (Phaseolus vulgaris L.) by near infrared spectroscopy

The presence of moisture, starch, protein, and fat was determined in common beans (Phaseolus vulgaris L.) by near infrared (NIR) spectroscopy without any previous sample pretreatment except grinding. A set of 96 samples was used to calibrate the instrument by modified partial least-squares regression. The following statistical results were achieved: standard error of calibration (SEC) = 0.31 and square correlation coefficient (R2) = 0.96 for moisture; SEC = 0.76 and R2 = 0.92 for starch; SEC = 0.39 and R2 = 0.98 for protein; and SEC = 0.14 and R2 = 0.80 for fat. To validate the calibration, a set of 25 bean samples was used. Standard errors of prediction were 0.39, 0.90, 0.56, and 0.13 for moisture, starch, protein, and fat, respectively, and R2 for the regression of measurements by the reference method versus NIR analysis were 0.94, 0.88, 0.94, and 0.74 for moisture, starch, protein, and fat, respectively. To compare the results obtained for all 4 components of the validation set by NIR spectroscopy with those obtained by the reference methods, linear regression and paired t tests were applied, and the methods did not give significantly different results, P = 0.05.     

基于灰狼算法的近红外光谱变量选择方法研究

基于群体智能的灰狼优化(GWO)算法具有参数少、结构简单、易于实现的优点,但在光谱领域的应用较少。该研究将GWO算法引入近红外光谱的变量筛选中,以玉米数据为例,考察了GWO算法中狼群性能、迭代次数、狼群数量及运算效率,并建立了偏最小二乘(PLS)模型对玉米样品中蛋白质、脂肪、水分以及淀粉含量的测定。结果显示,GWO算法运算效率很高,经过参数调优后建立PLS模型,其蛋白质、脂肪、水分及淀粉的保留变量数分别为19、19、14、34,预测均方根误差(RMSEP)从全波长PLS建模的0.245 8、0.122 4、0.339 8、1.105 8分别下降到0.147 7、0.080 1、0.176 2、0.739 8,分别下降了40%、35%、48%、33%,相关系数也相应地提高。因此,GWO算法不仅优化速度快,选择变量数少,还可以显著提高PLS模型的预测精度,是一种近红外光谱变量选择的有效方法。     

Use of NIRS technology with a remote reflectance fibre-optic probe for predicting major components in bee pollen

In the present work, we study the use of near infra-red spectroscopy (NIRS) technology together with a remote reflectance fibre-optic probe for determination of the major components in bee pollen. The method allows immediate control of the bee pollen without prior sample treatment or destruction through direct application of the fibre-optic probe to the sample.The regression method employed was modified partial least squares (MPLS). The calibration results obtained using 45 samples of bee pollen allowed the measurement of protein, moisture, ash, reducing sugars, and pH with multiple correlation coefficients (RSQ) and prediction corrected standard errors (SEPC) of 0.91, 0.56% for protein, of 0.78 and 0.49% for moisture; 0.92 and 0.049% for ash; 0.81 and 1.32 g of glucose/100 g of bee pollen; 0.84 and 0.15 for pH, respectively.The prediction capacity of the pattern was checked by applying it to samples of unknown pollen in external validation.     

Determination of fat, moisture, and protein in meat and meat products by using the FOSS FoodScan Near-Infrared Spectrophotometer with FOSS Artificial Neural Network Calibration Model and Associated Database: collaborative study

A collaborative study was conducted to evaluate the repeatability and reproducibility of the FOSS FoodScan near-infrared spectrophotometer with artificial neural network calibration model and database for the determination of fat, moisture, and protein in meat and meat products. Representative samples were homogenized by grinding according to AOAC Official Method 983.18. Approximately 180 g ground sample was placed in a 140 mm round sample dish, and the dish was placed in the FoodScan. The operator ID was entered, the meat product profile within the software was selected, and the scanning process was initiated by pressing the "start" button. Results were displayed for percent (g/100 g) fat, moisture, and protein. Ten blind duplicate samples were sent to 15 collaborators in the United States. The within-laboratory (repeatability) relative standard deviation (RSD(r)) ranged from 0.22 to 2.67% for fat, 0.23 to 0.92% for moisture, and 0.35 to 2.13% for protein. The between-laboratories (reproducibility) relative standard deviation (RSD(R)) ranged from 0.52 to 6.89% for fat, 0.39 to 1.55% for moisture, and 0.54 to 5.23% for protein. The method is recommended for Official First Action.     

Non-Invasive Method to Predict the Composition of Requeijão Cremoso Directly in Commercial Packages Using Time Domain NMR Relaxometry and Chemometrics

Low Field Time-Domain Nuclear Magnetic Resonance (TD-NMR) relaxometry was used to determine moisture, fat, and defatted dry matter contents in “requeijão cremoso” (RC) processed cheese directly in commercial packaged (plastic cups or tubes with approximately 200 g). Forty-five samples of commercial RC types (traditional, light, lactose-free, vegan, and fiber) were analyzed using longitudinal (T₁) and transverse (T₂) relaxation measurements in a wide bore Halbach magnet (0.23 T) with a 100 mm probe. The T₁ and T₂ analyses were performed using CWFP-T₁ (Continuous Wave Free Precession) and CPMG (Carr-Purcell-Meiboom-Gill) single shot pulses. The scores of the principal component analysis (PCA) of CWFP-T₁ and CPMG signals did not show clustering related to the RC types. Optimization by variable selection was carried out with ordered predictors selection (OPS), providing simpler and predictive partial least squares (PLS) calibration models. The best results were obtained with CWFP-T₁ data, with root-mean-square errors of prediction (RMSEP) of 1.38, 4.71, 3.28, and 3.00% for defatted dry mass, fat in the dry and wet matter, and moisture, respectively. Therefore, CWFP-T₁ data modeled with chemometrics can be a fast method to monitor the quality of RC directly in commercial packages.     

Infrared spectroscopy and outer product analysis for quantification of fat, nitrogen, and moisture of cocoa powder

The combination of the near infrared (NIR) and Fourier-transform infrared (FTIR) absorbance spectra (1100-2500 nm and 4000-600 cm⁻¹) of 100 cocoa powder samples was used to build calibration models for the determination of the content of fat, nitrogen, and moisture. The samples that comprised the dataset had an average composition of 13.51% of fat, 3.77% nitrogen, and 3.98% moisture. The fat content ranged from 2.42 to 22.00%, the nitrogen from 0.88 to 4.48%, and moisture from 1.60 to 7.80%. For NIR, the relative root mean square error of cross-validation (RMSECV) was 7.0% (R² = 0.96) for fat, 1.7% (R² = 0.98) for nitrogen, and 5.2% (R² = 0.94) for moisture. For FTIR, the relative RMSECV was 10.4% (R² = 0.94) for fat and 3.9% (R² = 0.95) for nitrogen. However, for moisture, it was not possible to build a calibration model with suitable predictability. The combination of the NIR and FTIR domains (data fusion) by outer product analysis PLS1 allowed to predict these parameters and to characterise frequencies in one domain based on the information of the other domain. This work allows to conclude that the second derivative of NIR is the recommended procedure to quantify fat, nitrogen, and moisture content in cocoa powders by infrared spectroscopy.     

Construction of an Isoperibol Calorimeter to Measure the Specific Heat Capacity of Foods Between 20 and 90°C

A simple isoperibol calorimeter, using the modified method of mixtures, was developed to measure the average specific heat capacity of different dough types between 20 and 90°C. The method consisted of encapsulating the sample in a copper cylinder and immersing the capsule in water at a different temperature. The procedure was tested for reliability with distilled water and whole fat milk before applying it to five dough types of varying moisture and fat contents. Mean values of 4.176±0.008 kJ kg^-1 K^-1 and 3.942±0.034 kJ kg^-1 K^-1 were obtained for distilled water and milk respectively, which agree within 0.23 and 0.34% from reported values. The specific heat values for the five dough types were found to range between 2.15–2.68 kJ kg^-1 K^-1 between 2.35–3.10 kJ kg^-1 K^-1 and between 2.40–3.19 kJ kg^-1 K^-1 at the three temperature levels studied. The specific heat capacity was found to depend not only on the moisture level but also on the fat content, especially for dough types with a high percent of fat. Regression analysis was then used to correlate these values and develop a set of empirical equations. The results were used to assist in energy balance calculations in backing oven for industrial purposes. This revised version was published online in July 2006 with corrections to the Cover Date.     

Long-term stability of nutrients in a frozen mixed food control material

A mixed food homogenate was prepared as a quality control material for two multi-center clinical feeding trials. Approximately 100 kg of homogenized human diet material was prepared under controlled conditions to maintain the stability of lipid components. More than 4,800 20-25 g aliquots were prepared and stored at -60 degrees C in glass jars with Teflon-lined lids. The homogeneity of the composite was validated by analysis of moisture and total fat in aliquots taken throughout the dispensing sequence. A portion of the material was reserved at the National Institute of Standards and Technology and further characterized as SRM 1544-Fatty Acids in Diet Composite. Moisture, protein, ash, total lipid, fatty acids, cholesterol, sodium, potassium, calcium, and magnesium were assayed as part of routine quality-control analyses. Components were analyzed over a total time period ranging from 29 months (minerals) to 60 months (moisture), and up to 319 values per nutrient were generated. Results for all components assayed were stable over the time period studied. For example, moisture (n = 319; 60 months) ranged from 70.66 to 72.58 g/100 g with a mean, standard deviation (SD), and relative standard deviation (RSD) of 71.90, 0.27, and 0.4%, respectively. The range, mean, SD, and RSD for cholesterol (mg/100 g; n = 98; 49 months) were 13.54-17.96, 15.14, 0.64, and 4%.     

Use of NIRS technology with a remote reflectance fibre-optic probe for predicting mineral composition (Ca,K, P,Fe, Mn,Na, Zn), protein and moisture in alfalfa

In the present work we study the use of near-infrared spectroscopy (NIRS) technology together with a remote reflectance fibre-optic probe for the analysis of major (Ca, K, P) and minor (Fe, Mn, Na, Zn) elements, protein and moisture in alfalfa. The method allows immediate analysis of the alfalfa without prior sample treatment or destruction through direct application of the fibre-optic probe on ground samples in the case of the mineral composition and on-ground and compacted (baled) samples in the case of protein and humidity. The regression method employed was modified partial least-squares (MPLS). The calibration results obtained using samples of alfalfa allowed the determination of Ca, K, P, Fe, Mn, Na and Zn, with a standard error of prediction (SEP(C)) and a correlation coefficient (RSQ) expressed in mg/kg of alfalfa of 1.37 × 10³ and 0.878 for Ca, 1.10 × 10³ and 0.899 for K, 227 and 0.909 for P, 103 and 0.948 for Fe, 5.1 and 0.843 for Mn, 86.2 and 0.979 for Na, and of 1.9 and 0.853 for Zn, respectively. The SEP(C) and RSQ values (in %) for protein and moisture in ground samples were 0.548 and 0.871 and 0.150 and 0.981, respectively; while in the compacted samples they were 0.564 and 0.826 and 0.262 and 0.935, respectively. The prediction capacity of the model and the robustness of the method were checked in the external validation in alfalfa samples of unknown composition, and the results confirmed the suitability of the method.     

Chemical characterization of "alcaparras" stoned table olives from northeast Portugal

Commercial stoned table olives named "alcaparras" from Trás-os-Montes (Portugal) were chemically characterized. During three consecutive years (2004-2006) 30 samples (10 per year) were examined for their nutritional value (moisture, crude protein, total fat, ash, carbohydrates, and energy), with a detailed report of the fatty acids and tocopherols composition. Water was the major constituent (72.5 ± 5.5%), followed by fat (14.6 ± 5.1%). The average amount of protein and ash were 1.1% and 3.4%, respectively, reporting unusual ash values for table olives, related to the technological process. One hundred grams of fresh stoned table olives presented an average energetic value of 156 kcal, lower than most table olives. The lipids are rich in oleic acid (average of 77.7 ± 2.0%), followed by palmitic acid and linoleic acid. Samples showed an average of total tocopherols of 1.2 mg/100 g of fresh weight, being α-tocopherol the most abundant. Table olives are important sources of MUFA, as olive oil, recognized as a preventive factor in diseases in which free radicals are implicated, complemented by the amounts of vitamin E, with both antioxidant and vitamin action.     

Near and mid-infrared photoacoustic analysis of principal components of foodstuffs

Photoacoustic spectroscopy, especially in the near infrared, for principal food component analysis (protein, fat, carbohydrate and moisture contents) is discussed. The thermal diffusion length is discussed as is the problem of signal saturation. An illustrative comparison of photoacoustic spectroscopy and Fourier transform mid-infrared-attenuated total reflectance spectroscopy (FTIR-ATR) as applied to cheese analysis is given.     

Ultrafiltration of Thin Stillage from Conventional and E-Mill Dry Grind Processes

We used ultrafiltration (UF) to evaluate membrane filtration characteristics of thin stillage and determine solids and nutrient compositions of filtered streams. To obtain thin stillage, corn was fermented using laboratory methods. UF experiments were conducted in batch mode under constant temperature and flow rate conditions. Two regenerated cellulose membranes (10 and 100 kDa molecular weight cutoffs) were evaluated with the objective of retaining solids as well as maximizing permeate flux. Optimum pressures for 10 and 100 kDa membranes were 207 and 69 kPa, respectively. Total solids, ash, and neutral detergent fiber contents of input TS streams of dry grind and E-Mill processes were similar; however, fat and protein contents were different (p < 0.05). Retentate obtained from conventional thin stillage fractionation had higher mean total solids contents (27.6% to 27.8%) compared to E-Mill (22.2% to 23.4%). Total solids in retentate streams were found similar to those from commercial evaporators used in industry (25% to 35% total solids). Fat contents of retentate streams ranged from 16.3% to 17.5% for the conventional process. A 2% increment in fat concentration was observed in the E-Mill retentate stream. Thin stillage ash content was reduced 60% in retentate streams.     

Highly active oxime-derived palladacycle complexes for Suzuki-Miyaura and Ullmann-type coupling reactions

Oxime-derived chloro-bridged palladacycles 12 and 13 are efficient complexes for the Suzuki-Miyaura reactions of aryl-, allyl-, and benzyl halides with arylboronic acids. The isolated catalysts are thermally stable, not sensitive to air or moisture, and easily accessible from inexpensive starting materials. The reaction can be performed under aerobic conditions with aryl bromides and chlorides, displaying turnover numbers (TON) of up to 5 x 10(5) and turnover frequencies (TOF) of up to 198 000 h(-1) for aryl bromides. Aryl chlorides undergo the Suzuki reaction with arylboronic acids with TON of up to 4700 and TOF up to 4700 h(-1). Even inexpensive and readily available benzyl and allyl chlorides undergo the coupling reaction with good turnover numbers. Complexes of 12 catalyze the syntheses of symmetrical biaryls in good yields via reductive coupling of iodoarenes in the presence of Hünig's base.     

Speciation of organotin compounds in marine sediments by capillary column gas chromatography-atomic absorption spectrometry coupled with hydride generation

A method for speciation of organotin compounds in marine sediments by solvent extraction combined with hydride generation gas chromatography-atomic absorption spectrometry has been developed. Sediment samples spiked with tributyltin and triphenyltin chlorides were homogenized in hydrochloric acid. The chlorides were extracted twice into toluene. Recoveries of the organotin compounds from the spiked sediment samples were improved by the addition of 8-quinolinol. Tributyltin and triphenyltin chlorides form ion-associates with 8-quinolinol in aqueous hydrochloric acid. The method was optimized with respect to derivatization reactions and extraction conditions. Interferences from Sn(II/IV) and additional 13 ions were investigated. Recoveries of 84-100% for tributyltin and 86-100% for triphenyltin were achieved using this method. The detection limits obtained for tributyltin and triphenyltin chlorides were 95 and 145 pg, respectively, corresponding to a relative detection limit of 95 and 145 ng kg(-1) in the sediment.     

Catalytic efficiency of a new tridentate ferrocenyl phosphine auxiliary: Sonogashira cross-coupling reactions of alkynes with aryl bromides and chlorides at low catalyst loadings of 10(-1) to 10(-4) mol %

[structure: see text] The catalytic activity in Sonogashira cross-coupling reactions of alkynes with a variety of aryl halides (including chlorides) using a multidentate ferrocenyl phosphine is presented. The novel mixed ferrocenyl aryl/alkyl triphosphine is thermally stable and insensitive to air or moisture, and its robustness allows aryl alkynylation at 10(-1) to 10(-4) mol % catalyst loadings with TONs up to 250,000. Copper-free coupling using phenylacetylene is also accessible in good yield.     

Determination of fat in dairy products using pressurized solvent extraction

Gravimetric fat data were obtained for a wide range of dairy products with fat contents ranging from 0.5 to 83% using pressurized solvent extraction at elevated temperatures and pressure (80-120 degrees C; 10.3 MPa). Extraction performance was sensitive to solvent composition, temperature, and sample matrix. By optimizing solvent mixtures, sample-solvent contact times of 8-10 min were sufficient for high recoveries from all products tested. The most successful solvents with regard to speed of extraction, selectivity, and recovery (average recovery, %) were various mixtures of hexane (or petroleum ether)-dichloromethane-methanol for dried cream (99.8%), dried whole milk (99.6%), dried buttermilk (98.2%), dried skim milk (97.0%), dried whey protein concentrate (97.5%), casein (95.0%), and caseinate (102.1%); petroleum ether-acetone-ethanol or petroleum ether-acetone-isopropanol for cheddar-type cheese (99.4%); petroleum ether-acetone for butter (99.9%); petroleum ether-acetone-isopropanol for cream (100.3%); and petroleum ether-isopropanol for liquid milks (99.0%). Relative standard deviations for repeatability were obtained for dried whole milk (0.2%), dried whey protein concentrate (0.7%), cheese (0.3%), butter (0.1%), and ultraheat treated (UHT) milk (0.7%). Solvent removal and drying of extracts with a heated block evaporator saved time compared with conventional drying ovens. Estimated savings in labor (50-75%) and solvents (80%) were substantial compared with the manual Mojonnier methods.