Luis E. Rodriguez-Saona

Rapid analysis of sugars in fruit juices by FT-NIR spectroscopy.

A simple analytical procedure using FT-NIR and multivariate techniques for the rapid determination of individual sugars in fruit juices was evaluated. Different NIR detection devices and sample preparation methods were tested by using model solutions to determine their analytical performance. Aqueous solutions of sugar mixtures (glucose, fructose, and sucrose; 0-8% w/v) were used to develop a calibration model. Direct measurements were made by transflection using a reflectance accessory, by transmittance using a 0.5-mm cell, and by reflectance using a fiberglass paper filter. FT-NIR spectral data were transformed to the second derivative. Partial least-squares regression (PLSR) was used to create calibration models that were cross-validated (leave-one-out approach). The prediction ability of the models was evaluated on fruit juices and compared with HPLC and standard enzymatic techniques. The PLSR loading spectra showed characteristic absorption bands for the different sugars. Models generated from transmittance spectra gave the best performance with standard error of prediction (SEP) <0.10% and R(2) of 99.9% that accurately and precisely predicted the sugar levels in juices, whereas lower precision was obtained with models generated from reflectance spectra. FT-NIR spectroscopy allowed for the rapid ( approximately 3 min analysis time), accurate and non-destructive analysis of sugars in juices and could be applied in quality control of beverages or to monitor for adulteration or contamination.

Influence of potato composition on chip color quality

Potato constituents were monitored to evaluate their contribution to potato chip color. Five chipping potato varieties: Snowden, AC Ptarmigan, FL 1625, FL 1815 and ND2471-8 were evaluated. Ascorbic acid, sugars, phenolic acids, and amino acids were determined and quantified by High Performance Liquid Chromatography (HPLC) and the color of potato chips was measured by both CIELab Hunter-ColorQuest and Agtron instruments. Composition and chip color varied among the different varieties. AC Ptarmigan and ND2471-8 produced the darkest chip color (on average L*= 49.0, chroma=19.5, and hue angle= 62.9) compared with FL 1815 (L*= 58.4, chroma= 28.3 and hue angle= 75.7). Reducing sugar concentration did not completely explain or predict color quality when it was present in low concentrations (ca. < 60 mg/100g). Other reactants present in the potato slices played an important role in the final color quality of potato chips. Multiple correlation analysis showed negative association of ascorbic acid (r= -0.7), fructose (r= -0.7), a chlorogenic acid isomer (r= -0.7), glucose (r= -0.7) and glutamine (r= -0.5) with potato chip color. Sucrose, chlorogenic acid and asparagine were poor estimators of chip color quality.ResumenDiferentes componentes de la papa fueron monitoreados para evaluar su contribucion en el desarrollo de color en papas fritas a la inglesa. Cinco variedades de papa para fritura: Snowden, AC Ptarmigan, FL 1625, FL 1815 y ND2471-8 fueron evaluadas. Acido ascórbico, azúcares, ácidos fenólicos y amino ácidos fueron determinados y cuantificados usando HPLC (cromatografía líquida de alta presión), y el color de las papas fritas fue medido usando los instrumentos CIELab Hunter ColorQuest y Agtron. Se encontró variabilidad en la composición y el color de las papas fritas obtenidas con las diferentes variedades de papa. AC Ptarmigan y ND2471-8 produjeron el color mas oscuro (en promedio L*=49.0, croma=19.5, y hue angle=62.9) comparado con FL 1815 (L*=58.4, croma=28.3 and hue angle=75.7). La concentration de azúcares reductores no fue suficiente para explicar o predecir la calidad del color final de las papas fritas a la inglesa, cuando estuvieron presentes en bajas concentraciones (aprox. < 60 mg/100g). Otros compuestos presentes en la papa desempeñaron un papel importante en color final de la papa frita. Análisis de correlaciones múltiples mostraron una asociación negativa entre el color obtenido y las concentraciones de ácido ascórbico (r=-0.7), fructosa (r=-0.7), un isómero del ácido clorogénico(r=-0.7), glucosa (r=-0.7) y glutamina (r=-0.5). El contenido de sucrosa, ácido clorogénico y asparagina no fueron buenos estimadores de la calidad del color final de la papa frita a la inglesa.

Rapid and Simultaneous Determination of Lycopene and β-Carotene Contents in Tomato Juice by Infrared Spectroscopy

The rapid quantification of lycopene and beta-carotene in tomato juices by attenuated total reflectance (ATR) infrared spectroscopy combined with multivariate analysis was evaluated. Two sample preparation methods were compared: a direct measurement of the tomato paste and an extraction method using hexane to isolate carotenoids. HPLC was used as the reference method. Cross-validated (leave-one-out) partial least-squares regression (PLSR) was used to create calibration models to predict these phytonutrient concentrations in blind test samples. The infrared spectra showed unique marker bands at 957 and 968 cm(-1) for lycopene and beta-carotene, respectively. Multivariate analysis of the infrared spectral data gave correlation coefficients (r values) of >0.9 between the ATR-IR predicted and HPLC reference values, and standard errors of cross-validation (SECV) of 0.5 and 0.04 mg/100 g of juice for lycopene and beta-carotene, respectively. ATR-IR could provide the tomato industry with a simple, rapid, and high-throughput technique for the determination of tomato quality.

Application of hand-held and portable infrared spectrometers in bovine milk analysis.

A simple and fast method for the detection and quantification of milk adulteration was developed using portable and hand-held infrared (IR) spectrometers. Milk samples were purchased from local supermarkets (Columbus, OH, USA) and spiked with tap water, whey, hydrogen peroxide, synthetic urine, urea, and synthetic milk in different concentrations. Spectral data were collected using mid-infrared (MIR) and near-infrared (NIR) spectrometers. Soft independent modeling of class analogy (SIMCA) classification models exhibited tight and well-separated clusters allowing the discrimination of control from adulterated milk samples. Partial least-squares regression (PLSR) was used to estimate adulteration levels, and results showed high coefficients of determination (R(2)) and low standard errors of prediction (SEP). Classification and quantification models indicated that the tested MIR systems were superior to NIR systems in monitoring milk adulteration. This method can be potentially used as an alternative to traditional methods due to their simplicity, sensitivity, low energy cost, and portability.

Purification and identification of capulin (Prunus serotina Ehrh) anthocyanins

Abstract Capulin (Prunus serotina Ehrh) anthocyanins were extracted from liquid nitrogen powdered epidermal tissue using acetone, the aqueous acetone extract partitioned with chloroform and purified in a C-18 solid-phase cartridge. pH-differential and bisulfite bleaching methods were used to determine monomeric anthocyanin content and polymeric color. Pigments were identified by spectral analyses, HPLC and mass spectroscopy. Information from HPLC profiles, saponification and acid hydrolysis of the capulin anthocyanins showed that the two major pigments were cyanidin-3-glucoside (34%) and cyanidin-3-rutinoside (63%), with no acylating groups. A third yellow/orange pigment (λmax 480 nm, MW=632) possibly containing rutinose was detected by MS.

Rapid detection and differentiation of Alicyclobacillus species in fruit juice using hydrophobic grid membranes and attenuated total reflectance infrared microspectroscopy.

Pasteurized juices may undergo spoilage during normal shelf life due to Alicyclobacillus spp. Metabolic byproducts during germination of these thermoacidiophilic, endospore-forming bacteria impart off-flavors. The objective was to develop a simple, rapid, and sensitive approach for differentiation of Alicyclobacillus spp. by attenuated total reflectance infrared (ATR-IR) microspectroscopy after isolation onto hydrophobic grid membrane (HGM) filters. Dilutions of four different species of Alicyclobacillus were filtered onto HGM, incubated on orange serum agar (50 degrees C, 36-48 h), and dried under vacuum. Spectra were collected using ATR-IR microspectroscopy and analyzed by multivariate analysis. Results indicated that soft independent modeling of class analogy models exhibited clusters that permitted classification at species and strain levels. The methodology was validated by correctly predicting Alicyclobacillus (100%) in blind tests. The proposed procedure permits chemically based classification of intact microbial cells. Implementation provides the juice industry with a rapid screening procedure to detect and monitor Alicyclobacillus that threatens the quality of pasteurized juices.

Carotenoid stability during production and storage of tomato juice made from tomatoes with diverse pigment profiles measured by infrared spectroscopy.

Chemical changes in carotenoids and lipids were studied during production and storage of canned tomato juice using ATR infrared spectroscopy and HPLC. Samples from 10 groups of tomatoes with different carotenoid profiles were analyzed fresh, after hot-break and screening, after canning, and at five different time points during 1 year of storage. An apparent increase of carotenoids was observed after hot-break due to improved extraction efficiency. This increase was accompanied by some degree of lipid oxidation and carotenoid isomerization. Canning produced the most intense changes in the lipid profile with breakdown of triglycerides ( approximately 1743 cm(-1)), formation of fatty acids ( approximately 1712 cm(-1)), and degradation and isomerization of trans-carotenoids ( approximately 960 and approximately 3006 cm(-1)). Isomerization was corroborated by the relative increase of HPLC areas corresponding to carotenoid cis isomers. Canning reduced trans-lycopene, trans-delta-carotene, trans-beta-carotene, and trans-lutein by 30, 34, 43, and 67%, respectively. HPLC data indicate that canning causes a drastic reduction of tetra-cis-lycopene and promotes its isomerization to other geometric forms, including all-trans-lycopene. Infrared spectra of tomato juice lipid fractions correlated well with the number of days in storage (SECV < 11 days, r values > 0.99), demonstrating continuous degradation of lipids. Results demonstrated that individual carotenoids and their isomeric forms behave differently during production and storage of canned tomato juice. Information collected by infrared spectroscopy complemented well that of HPLC, providing marker bands to further the understanding of chemical changes taking place during processing and storage of tomato juice.

Improving the Screening Process for the Selection of Potato Breeding Lines with Enhanced Polyphenolics Content

Efficient selection of potato varieties with enhanced nutritional quality requires simple, rapid, accurate, and cost-effective assays to obtain tuber chemical composition information. Our objective was to develop simple protocols to determine phenolics, anthocyanins, and antioxidant capacity in polyphenolic extracts of potatoes using Fourier transform infrared spectroscopy combined with multivariate techniques. Lyophilized potato samples (23) were analyzed. Polyphenolic compounds were extracted from potatoes and applied directly applied onto a three-bounce ZnSe crystal for attenuated total reflectance measurements in the infrared region of 4000 to 700 cm (-1). Robust models were generated (r > or = 0.99) with standard error of cross-validation values of 4.17 mg gallic acid equivalent/100 g (total phenolics), 0.87 mg pelargonidin-3-glucoside/100 g (monomeric anthocyanins), and 130.8 mumol Trolox equivalent/100 g (antioxidant capacity) potato powder. In addition, classification models discriminated potato samples at the species and variety level. Application of a simple infrared spectroscopic protocol allowed simultaneous rapid quantification of specific nutritional components in potatoes and efficient selection of value-added potato varieties.