Rapid determination of moisture/solids and fat in dairy products by microwave and nuclear magnetic resonance analysis

A peer-verified method is presented for the determination of percent moisture/solids and fat in dairy products by microwave drying and nuclear magnetic resonance (NMR) analysis. The method involves determining the moisture/solids content of dairy samples by microwave drying and using the dried sample to determine the fat content by NMR analysis. Both the submitting and peer laboratories analyzed various dairy products by using a CEM SMART system (moisture) and the SMART Trac (fat). The samples included milks, creams, ice cream mix, sour cream, yogurt, cream cheese, and mozzarella, Swiss, and cheddar cheeses. These samples represented a range of products that processors deal with in daily plant operations. The results were compared with moisture/solids and fat values derived from AOAC-approved methods.     

Determination of moisture and fat in meats by microwave and nuclear magnetic resonance analysis: collaborative study

Ten laboratories participated in a collaborative study to determine the total moisture and fat in raw and processed meat products by microwave drying and nuclear magnetic resonance (NMR) spectroscopy. Meat products were prepared following the AOAC Method and analyzed using CEM Corp.'s SMART Trac Moisture and Fat Analysis system. SMART Trac provides moisture results by measuring the weight loss on drying by microwave energy. The dried sample is then analyzed by NMR spectrometry for fat content. Moisture and fat results are displayed and reported by the SMART Trac as a percentage (g/100 g). Microwave drying is an AOAC-approved reference method (Method 985.14), Moisture in Meat and Poultry Products. NMR spectrometry is a secondary technique used to determine the concentration of various constituents in biological, organic, or chemical samples. The study design was based on Youden's matched pair principle for collaborative tests. For the purposes of this study, 10 laboratories each tested 10 Youden matched pairs, for a total of 20 samples. The study samples represented a range of products processed daily in plant operations. Included were raw meat samples (beef, pork, chicken, and turkey) as well as processed meats (beef hot dog, pork sausage, and ham). The total moisture content of the undiluted samples, as received for the purposes of this study, was determined by AOAC Method 950.46 and ranged from 54.03 to 74.99%. The total fat content of the undiluted samples was determined by AOAC Method 960.39 and ranged from 1.00 to 29.79%. Statistical analysis of study results for total moisture yielded a relative standard deviation for repeatability (RSDr) range of 0.14 to 0.95% and a relative standard deviation for reproducibility (RSDR) range of 0.26 to 0.95%. Statistical analysis for total fat yielded similar RSDr and RSDR range of 0.74 to 4.08%. Results for turkey had higher RSDr and RSDR values, both at 12.6%, due to low fat content and possibly to the separation of the samples observed by some of the collaborators. Results demonstrate that microwave drying with NMR is a rapid, practical method providing results equivalent to AOAC Methods 950.46 (Forced Air Oven Drying) and 960.39 (Soxhlet Ether Extraction) in raw and processed meat products.     

Determination of crude fat in meat by supercritical fluid extraction: direct method: PVM 3:2000

Meat samples are prepared by passing meat through a food chopper, bowl cutter, or food processor, subsampling the meat, and mixing the meat with granular diatomaceous earth. No drying step is necessary. Supercritical CO2 is then used to extract crude fat (which is defined as the components of meat that are extractable with petroleum ether, without digestion of the sample). Extracted material is deposited on glass wool contained in collection vials. After removal of any residual moisture from the extracts, percent crude fat is determined by weight gain of the collection vial. This method has been peer-verified by 3 laboratories, for a wide variety of raw and processed meat products containing 6-28% crude fat. Samples were prepared at the submitting laboratory. Ground samples were split into 4 portions, packed in Whirlpack bags, and immediately frozen. Frozen samples were sent by overnight room temperature, and percent fat was determined (in triplicate), without further processing of the samples. Analysis of the samples was completed within 1 week of sample prepara. tion. On the basis of this study, it can be estimated that all repeatability and reproducibility values are <3.0. Mean accuracy of the direct gravimetric supercritical fluid extraction method for meat samples ranged from +0.22 to -1.41 when the method was compared with AOAC Method 960.39. Interferences are unlikely but would include any nonfat substance that is added to (processed) meat, is soluble in nonpolar solvents, and is present in a quantity that would alter results. This method is expected to perform equally well for all meats with fat content within the stated range of applicability.     

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.     

Effect of Different Drying Methods on the Nutritional Value of Hibiscus sabdariffa Calyces as Revealed by NMR Metabolomics

Red mature calyces of Hibiscus sabdariffa were collected from 16 different locations in Meghalaya, India. Samples were processed using shade drying (SD) and tray drying (TD). NMR spectroscopy was used to assess the metabolic composition of the calyces. In this study, 18 polar metabolites were assigned using 1D and 2D NMR spectra, and 10 of them were quantified. Proximate analysis showed that the TD method is more efficient at reducing moisture and maintaining the ash content of the Hibiscus biomass. NMR metabolomics indicates that the metabolite composition significantly differs between SD and TD samples and is more stable in TD plant processing. The differences in post-harvest drying has a greater impact on the metabolite composition of Hibiscus than the plant location.     

Effects of drying and pressing on the pore structure in the cellulose fibre wall studied by 1H and 2H NMR relaxation

A 1H and 2H NMR relaxation method was used to investigate the influence of drying and pressing on the pore size and pore size distribution in the cellulose fibre wall. The investigation was made in the moisture interval in which cellulose fibres normally shrink, i.e. from a moisture ratio of about 1.5 g water/g fibre to dry fibres. When the moisture content of a fibre sample was decreased by drying or pressing, the pores decreased in size and the pore size distribution became narrower. It was found that there were only small differences at a given moisture content between the pore size distributions of samples prepared by drying and by pressing. The results also indicate that the pore shrinkage in cellulose fibres during pressing or drying is a process in which the cell wall pores of a wet cellulose fibre successively shrink as the moisture content decreases. It was observed that, at low moisture contents, pressing and drying resulted in different 1H NMR spin-lattice relaxation profiles. This is discussed in terms of morphology differences in the fibre matrix. The mobility of the protons in the solid phase influences the liquid 1H NMR spin-lattice relaxation in heterogeneous systems through magnetization transfer. We have also studied the effects of hornification in recycled pulps     

Determination of nitrite, nitrate, and glucose-6-phosphate in muscle tissues and cured meat by IC/MS

The endogenous nitrate concentration in fresh meat and the residual nitrate and nitrite contents after curing are related to food quality and safety. Most ion chromatography (IC) methods suffer from interferences, especially in fresh meat samples, in which the endogenous nitrate content is low, and in cured meat products, in which other nitrogenous compounds can interfere with the separation of inorganic anions. One of the major classes of interfering compounds in fresh meat are sugar phosphates, which originate from glycolysis during the conversion of muscle glycogen to lactic acid. Nitrate can be separated from interfering compounds with a high-capacity anion-exchange column that was manufactured for use with hydroxide eluents (i.e., hydroxide-selective). This column has a different selectivity than traditional IC columns that use carbonate eluents and facilitates the determination of nitrate in both fresh and cured meats. Nitrate was detected by both suppressed conductivity measurement and mass spectrometry (MS). The identifications of nitrate and glucose-6-phosphate were confirmed by MS detection. The described IC/MS method is robust, sensitive to nitrate concentrations as low as 0.10 mg/kg, and can determine sugar phosphates that are useful for monitoring meat freshness. We successfully used this method to determine nitrate in nearly 100 muscle tissues and cured meat samples.     

肉类制品中微量锶的分离及^87Sr/^86Sr同位素比值测定

利用87Sr/86Sr同位素比值进行生物和古人类源区与迁徙的示踪是Sr同位素技术应用的新领域,也是考古研究和肉类食品溯源研究的新尝试。本研究对牛肉干粉采用酸溶、微波消解和灰化后硝酸提取等不同方法进行消解,比较了它们的离子交换分离效果和Sr同位素测定结果;用石英、石墨和瓷坩埚3种器皿对牛肉干粉进行灰化,检测了灰化器皿对87Sr/86Sr同位素比值的影响,从而确定了石英坩埚灰化的消解方法,建立了适合于肉类制品微量Sr的化学分离方法与87Sr/86Sr同位素比值测定方法。本方法包括肉类制品的石英坩埚灰化、离子交换分离和87Sr/86Sr比值的热离子化质谱测定。所建方法对肉类食品溯源和考古研究等领域富含有机质样品的Sr同位素比值测定具有普适性。     

NIR-spectrometric analysis of food. Methodical development and achievable performance values

The application of near infrared spectrometry (NIRS) to estimate the distribution of macro nutrients in food provides a rapid method for predicting food quality. Three methods have been developed for quantitative determination of the constituents of foods containing high levels of moisture (meat products, “consumable meals” and potatoes) using reflectance spectrometry in the near infrared region within 1100–2500 nm. Experience concerning these NIRS method developments is reported in order to predict e.g. the fat, crude protein and carbohydrate content. Generally, the performance values achieved so far indicate that the methods may be used as a replacement for conventional expensive and time-consuming wet chemical analysis.     

Changes in Physicochemical Properties and Volatile Compounds of Roselle (Hibiscus sabdariffa L.) Calyx during Different Drying Methods

Fresh roselle are high in moisture and deteriorate easily, which makes drying important for extending shelf-life and increasing availability. This study investigated the influence of different drying methods (oven-drying, freeze-drying, vacuum-drying, and sun-drying) on the quality of roselle calyx expressed as physicochemical properties (moisture content, water activity, soluble solids, color), volatile compounds, and microstructure. Oven-drying and freeze-drying reduced moisture content most while vacuum-drying and sun-drying were not as efficient. All drying methods except sun-drying resulted in water activities low enough to ensure safety and quality. Vacuum-drying had no impact on color of the dry calyx and only small impact on color of water extract of calyx. Drying reduced terpenes, aldehydes, and esters but increased furans. This is expected to reduce fruity, floral, spicy, and green odors and increase caramel-like aroma. Sun-drying produced more ketones, alcohols, and esters. Scanning electron microscopy revealed that freeze-drying preserved the cell structure better, and freeze-dried samples resembled fresh samples most compared to other drying techniques. The study concludes that freeze-drying should be considered as a suitable drying method, especially with respect to preservation of structure.     

Analysis and aging of unsaturated polyester resins in contemporary art installations by NMR spectroscopy

Two original art installations constructed from unsaturated polyester resins (UPR) and four different reference UPR products (before and after UVB aging) were analyzed by high-resolution 1D and 2D nuclear magnetic resonance (NMR) spectroscopy. Breaking strain studies were also conducted for the four UPR model products before and after different aging procedures (moisture, UVB exposure, melt/freeze). NMR analysis of the chemical composition of the UPR resin extracts showed they contain several low MW organic compounds and oligomers rich in polar -OH groups that play a significant role in the degradation behavior of the composite UPR materials. Statistical analysis of the NMR compositional data showed that styrene and benzaldehyde contents can be used to differentiate between fresh and aged UPR samples. The phthalate and propylene glycol unit speciation (esterified, primary or secondary -OH) of the extracts provided evidence that UPR resin C was used in the construction of the two art installations, and direct comparison of (1)H and (13)C NMR spectra verified this compositional similarity. UPR resin C was shown by both NMR and breaking strain studies to be the reference UPR most susceptible to degradation by different aging procedures, a characteristic attributed to the lower styrene content of resin C.     

Microwave drying of granules containing a moisture-sensitive drug: a promising alternative to fluid bed and hot air oven drying

The impact of microwave drying and binders (copolyvidone and povidone) on the degradation of acetylsalicylic acid (ASA) and physical properties of granules were compared with conventional drying methods. Moist granules containing ASA were prepared using a high shear granulator and dried with hot air oven, fluid bed or microwave (static or dynamic bed) dryers. Percent ASA degradation, size and size distribution, friability and flow properties of the granules were determined. Granules dried with the dynamic bed microwave dryer showed the least amount of ASA degradation, followed by fluid bed dryer, static bed microwave oven and hot air oven. The use of microwave drying with a static granular bed adversely affected ASA degradation and drying capability. Dynamic bed microwave dryer had the highest drying capability followed by fluid bed, static bed microwave dryer and conventional hot air oven. The intensity of microwave did not affect ASA degradation, size distribution, friability and flow properties of the granules. Mixing/agitating of granules during drying affected the granular physical properties studied. Copolyvidone resulted in lower amount of granular residual moisture content and ASA degradation on storage than povidone, especially for static bed microwave drying. In conclusion, microwave drying technology has been shown to be a promising alternative for drying granules containing a moisture-sensitive drug.     

Determination of phosphate compounds in meat products by 31-Phosphorus Nuclear Magnetic Resonance spectroscopy with methylenediphosphonic acid after alkaline extraction

Modification of the extraction procedure and application of the ³¹P NMR method for the determination of polyphosphates in meat products were studied. In the elaborated procedure threefold water extraction at alkaline pH (borate buffer and 0.1 M EDTA) was applied. Furthermore, the new external standard for ³¹P NMR determination of phosphates was proposed. Obtained recoveries were between 95 and 99% and variation coefficients (CV) was ≤5%, indicating an increase in accuracy and the precision of the proposed procedure in relation to the spectrophotometric method. The described procedure of sample preparation with ³¹P NMR method was applied for the determination of polyphosphate additives in meat products. The satisfactory precision (CV = 0.39-3.40%) shows the benefit of the NMR method in the routine analysis of the phosphate ions in meat products.     

Water Status and Predictive Models of Moisture Content during Drying of Soybean Dregs Based on LF-NMR

To explore the drying characteristics of soybean dregs and a nondestructive moisture content test method, in this study, soybean dregs were dried with hot air (80 °C), the moisture content was measured using the drying method, water status was analyzed using low-field nuclear magnetic resonance (LF-NMR) and the moisture content prediction models were built and validated. The results revealed that the moisture contents of the soybean dregs were 0.57 and 0.01 g/g(w.b.), respectively, after drying for 5 and 7 h. The effective moisture diffusivity increased with the decrease in moisture content; it ranged from 5.27 × 10⁻⁹ to 6.96 × 10⁻⁸ m²·s⁻¹. Soybean dregs contained bound water (T₂₁), immobilized water (T₂₂) and free water (T₂₃ and T₂₃’). With the proceeding of drying, all of the relaxation peaks shifted left until a new peak (T₂₃’) appeared; then, the structure of soybean dregs changed, and the relaxation peaks reformed, and the peak shifted left again. The peak area may predict the moisture content of soybean dregs, and the gray values of images predict the moisture contents mainly composed of free water or immobilized water. The results may provide a reference for drying of soybean dregs and a new moisture detection method.     

Fat content for nutritional labeling by supercritical fluid extraction and an on-line lipase catalyzed reaction

A method using sequential supercritical fluid extraction (SFE) and enzymatic transesterification has been developed for the rapid determination of total nutritional fat content in meat samples. SFE conditions of 12.16 MPa and 50°C were utilized to extract lipid species from the sample matrix. The enzymatic transesterification of the lipids by methanol was catalyzed by an immobilized lipase isolated from Candida antarctica. Conversion of the triglycerides to fatty acid methyl esters was monitored by supercritical fluid chromatography, while the fatty acid content of the extract was determined by capillary gas chromatography (GC). Total fat, saturated fat and monounsaturated fat contents were calculated from the GC data and compared to values from traditional extraction and lipid determination methods. Both off-line SFE and automated SFE followed by on-line GC analysis using two different instruments were utilized in this study. The enzymatic-based SFE method gave comparable results to the organic solvent extraction-based method followed by conventional BF₃-catalyzed esterification.     

A preliminary study of milk powder hydration using TEDSpiL continuous wave NMR

Moisture content of foodstuffs are typically assessed by Titration or Near Infrared Spectroscopy, which are labour-intensive as a manual measurement or costly when automated. Magnetic resonance offers a method for moisture evaluation but is also normally costly. In this work, we revisit Look and Locker's “Tone Burst” experiment with a marginal oscillator to evaluate moisture content of powdered–skimmed milk subjected to increased humidity. We refer to this technique as the Transient Effect Determination of Spin–Lattice (TEDSpiL) relaxation times. Moisture content in the samples ranged from 0–12% as determined from the weight gained by the dry powder when re-suspended in water to reach a concentration of 40% w/v. The relaxation properties of re-hydrated samples were measured with a CW NMR sensor. Solutions made up from powders with a higher retained moisture content provided lower measured relaxation values providing a method of measuring the moisture content of the powder. This technique provides a moisture measurement in under 5∼s compared with several minutes for the equivalent pulsed method using low-field hardware.     

A clean up step of fat content previous to trace metal characterization in mussel tissues by inductively coupled plasma mass spectrometry

Inductively coupled plasma mass spectrometry analysis of trace and major elements of mussel tissues can be quickly and accurately analyzed after cleaning up the interfering fat content before the sample is digested in a microwave oven. Making use of experimental designs, the clean up procedure was achieved by the extraction of 1 g of freeze-dried tissue sample stirred with 5 ml of dichloromethane during five minutes. The microwave assisted digestion of the fat free samples was carried out with 0.2 g of tissue sample, 15 ml of 7.0% nitric acid with a power of 980 W during 18 min. The analytical method efficiency (accuracy and precision) was evaluated with a CRM: (NIST 2977, mussel tissue) and real mussel samples analyzed previously. The results confirmed the accuracy of the analysis by agreement with the previous results but the precision was significantly improved. The developed method allows operating routinely permitting to large numbers of samples to be quickly screened for trace metals.     

The Quality of Infrared Rotary Dried Terebinth (Pistacia atlantica L.)-Optimization and Prediction Approach Using Response Surface Methodology

Most agricultural products are harvested with a moisture content that is not suitable for storage. Therefore, the products are subjected to a drying process to prevent spoilage. This study evaluates an infrared rotary dryer (IRRD) with three levels of infrared power (250, 500, and 750 W) and three levels of rotation speed (5, 10, and 15 rpm) to dry terebinth. Response surface methodology (RSM) was used to illustrate and optimize the interaction between the independent variables (infrared power and rotation speed) and the response variables (drying time, moisture diffusivity, shrinkage, color change, rehydration rate, total phenolic content, and antioxidant activity). As infrared power and rotation speed increased, drying time, rehydration rate, antioxidant activity, and total phenolic content decreased, while the other parameters were increased. According to the results, the optimum drying conditions of terebinth were determined in the IRRD at an infrared power of 250 W and drum rotation speed of 5 rpm. The optimum values of the response variables were 49.5 min for drying time, 8.27 × 10⁻⁹ m²/s for effective moisture diffusivity, 2.26 for lightness, 21.60 for total color changes, 34.75% for shrinkage, 2.4 for rehydration rate, 124.76 mg GAE/g d.m. for total phenolic content and 81% for antioxidant activity.