High pressure liquid chromatographic determination of antihistamine-adrenergic combination products: collaborative study

A reverse phase high pressure liquid chromatographic method in which ion-pairing is used for the determination of combinations of pseudoephedrine hydrochloride with triprolidine hydrochloride or chlorpheniramine maleate in syrups and tablets was collaboratively studied by 8 laboratories. Collaborators were supplied with 12 samples including synthetic and commercial syrup formulations and commercial tablet composites. Mean recoveries of pseudoephedrine hydrochloride and triprolidine hydrochloride from synthetic syrup formulations were 100.5 and 99.6%, respectively. Mean recoveries of pseudoephedrine hydrochloride and chlorpheniramine maleate from synthetic syrups were 98.8 and 100.5%, respectively. Mean coefficients of variation for syrups and tablets ranged from 1.68 to 3.07% for pseudoephedrine hydrochloride, from 2.92 to 3.85% for triprolidine hydrochloride, and from 1.34 to 2.15% for chlorpheniramine maleate. The method has been adopted official first action.     

Liquid chromatographic methods for vitamins A and D in multivitamin-mineral formulations

Liquid chromatographic screening procedures have been developed for the estimation of vitamins A and D in multivitamin-mineral tablet, capsule, gelatin capsule, and syrup formulations. The procedure can be used for measuring vitamin A present as either retinyl acetate or retinyl palmitate, and also for measuring the contribution to total vitamin A activity from 13-cis retinyl esters. The retinyl esters and their isomers are resolved from each other and their oxidation products. Ergocalciferol and cholecalciferol are not resolved from each other but they are resolved from other vitamin D isomers and from vitamins A, E, and K and their degradation products. Both assays use a 3 microns amino column, with a mobile phase of hexane for vitamin A and 1% isopropanol in hexane for vitamin D. The precision of replicate injections for vitamins A and D is better than 1% and the recovery from spiked syrups is better than 98%. The coefficient of variation for both assay methods is about 5%. Twenty formulations were analyzed for vitamin A and 24 were analyzed for vitamin D.     

Liquid chromatography/mass spectrometry investigation of the impact of thermal processing and storage on peach procyanidins

Normal-phase liquid chromatography/mass spectrometry (LC/MS) was used to determine the levels and fate of procyanidins in frozen and canned Ross clingstone peaches as well as in the syrup used in the canning over a 3 month period. Procyanidin oligomers, monomers through undecamers, were identified in Ross clingstone peaches. Optimized methods allowed for the quantitation of oligomers through octamers. The profile of procyanidins in peaches is similar to profiles found in grapes, chocolate, and beverages linked to health benefits such as tea and wine. The monomer content in frozen peeled peaches was found to be 19.59 mg/kg. Dimers (39.59 mg/kg) and trimers (38.81 mg/kg) constituted the largest percent composition of oligomers in the peaches. Tetramers through octamers were present in levels of 17.81, 12.43, 10.62, 3.94 and 1.75 mg/kg, respectively. Thermal processing resulted in an 11% reduction in monomers, a 9% reduction in dimers, a 12% reduction in trimers, a 6% reduction in tetramers, and a 5% reduction in pentamers. Hexamers and heptamers demonstrated an approximate 30% loss, and octamers were no longer detected. Analysis of the syrup after thermal processing indicates that there is a migration of procyanidin monomers through hexamers into the syrup that can account for the losses observed during the canning process. Storage of canned peaches for 3 months demonstrated a time-related loss in higher oligomers and that by 3 months oligomers larger than tetramers are not observed. At 3 months postcanning, levels of monomers had decreased by 10%, dimers by 16%, trimers by 45%, and tetramers by 80%. A similar trend was observed in the canning syrup.     

Improved detection of sugar addition to maple syrup using malic acid as internal standard and in 13C isotope ratio mass spectrometry (IRMS)

Stable carbon isotope ratio mass spectrometry (delta13C IRMS) was used to detect maple syrup adulteration by exogenous sugar addition (beet and cane sugar). Malic acid present in maple syrup is proposed as an isotopic internal standard to improve actual adulteration detection levels. A lead precipitation method has been modified to isolate quantitatively malic acid from maple syrup using preparative reversed-phase liquid chromatography. The stable carbon isotopic ratio of malic acid isolated from this procedure shows an excellent accuracy and repeatability of 0.01 and 0.1 per thousand respectively, confirming that the modified lead precipitation method is an isotopic fractionation-free process. A new approach is proposed to detect adulteration based on the correlation existing between the delta13Cmalic acid and the delta13Csugars-delta13Cmalic acid (r = 0.704). This technique has been tested on a set of 56 authentic maple syrup samples. Additionally, authentic samples were spiked with exogeneous sugars. The mean theoretical detection level was statistically lowered using this technique in comparison with the usual two-standard deviation approach, especially when maple syrup is adulterated with beet sugar : 24 +/- 12% of adulteration detection versus 48 +/- 20% (t-test, p = 7.3 x 10-15). The method was also applied to published data for pineapple juices and honey with the same improvement.     

Specific screening for color precursors and colorants in beet and cane sugar liquors in relation to model colorants using spectrofluorometry evaluated by HPLC and multiway data analysis

A comparison was made of the fluorophores in beet thick juice and cane final evaporator syrup, which are comparable in the production of cane and beet sugar; that is, both represent the final stage of syrup concentration prior to crystallization of sugar. To further elucidate the nature of the color components in cane and beet syrup, a series of model colorants was also prepared, consisting of mildly alkaline-degraded fructose and glucose and two Maillard type colorants, glucose--glycine and glucose--lysine. Fluorescence excitation--emission landscapes resolved into individual fluorescent components with PARAFAC modeling were used as a screening method for colorants, and the method was validated with size exclusion chromatography using a diode array UV--vis detector. Fluorophores from the model colorants were mainly located at visible wavelengths. An overall similarity in chromatograms and absorption spectra of the four model colorant samples indicated that the formation of darker color was the distinguishing characteristic, rather than different reaction products. The fluorophores obtained from the beet and cane syrups consisted of color precursor amino acids in the UV wavelength region. Tryptophan was found in both beet and cane syrups. Tyrosine as a fluorophore was resolved in only beet syrup, reflecting the higher levels of amino acids in beet processing. In the visible wavelength region, cane syrup colorant fluorophores were situated at higher wavelengths than those of beet syrup, indicating formation of darker colorants. A higher level of invert sugar in cane processing compared to beet processing was suggested as a possible explanation for the darker colorants.     

Beet sugar syrup and molasses as low-cost feedstock for the enzymatic production of fructo-oligosaccharides

Sugar syrup and molasses from beet processing containing 620 and 570 mg/mL sucrose, respectively, were assayed as low-cost and available substrates for the enzymatic synthesis of fructo-oligosaccharides (FOSs). A commercial pectinase (Pectinex Ultra SP-L, from Aspergillus aculeatus) characterized by the presence of a transfructosylating activity was used as a biocatalyst. The FOS production increased when lowering the initial pH value of syrup (7.5) and molasses (8.9) to 5.5. Sugar syrup and molasses were diluted in order to reduce substrate viscosity; interestingly, the percentage of FOS with regards to total sugars remained almost constant, which indicated a high transferase-to-hydrolase ratio for this enzyme. Kinetics of FOS production was analyzed. Using approximately 10 U transfructosylating activity per g sucrose, the FOS concentration reached a maximum of 388 mg/mL after 30 h using syrup and 235 mg/mL in 65 h with molasses. These values corresponded to approximately 56 and 49% (w/w), respectively, of the total amount of carbohydrates in the mixture. The enzyme was also covalently immobilized on an epoxy-activated polymethacrylate-based polymer (Sepabeads EC-EP5). We found that immobilized Pectinex Ultra SP-L can be efficiently applied to the synthesis of FOS using syrup and molasses as substrates.     

Spray-dried multilayered emulsions as a delivery method for omega-3 fatty acids into food systems

Emulsion can be produced with electrostatic layer-by-layer deposition technologies to have cationic, thick multilayer interfacial membranes that are effective at inhibiting the oxidation of omega-3 fatty acids. This study investigated the stability of spray-dried multilayer emulsion upon reconstitution into an aqueous system. The primary (lecithin) and multilayered secondary emulsions (lecithin and chitosan) were spray-dried with corn syrup solids (1-20 wt %). The lecithin-chitosan multilayer interfacial membrane remained intact on the emulsion droplets upon reconstitution into an aqueous system. Reconstituted secondary (lecithin-chitosan) emulsions were more oxidatively stable than reconstituted primary (lecithin) emulsions. A minimum of 5 wt % corn syrup solids was needed to microencapsulate the secondary emulsion droplets. Maximum oxidative stability of both the powder and the reconstituted secondary emulsions was observed in samples with 5% and 20% corn syrup solids. Addition of EDTA (25 microM) inhibited oxidation of reconstituted primary and secondary emulsions. These studies suggest that a microencapsulated multilayered emulsion system could be used as a delivery system for omega-3 fatty acids in functional foods.     

Formulations of controlled atmosphere agents for packaged foods.

Four food grade additives-sodium ascorbate, sodium bicarbonate, sodium carbonate-10-hydrate, and ferrous sulfate-7-hydrate-were selected as the basic ingredients to formulate the controlled atmosphere agents which could effectively remove oxygen and release carbon dioxide. The mathematical models giving the relationships between the formulations and the responses (oxygen and carbon dioxide contents) were developed using response surface methodology (RSM). Within 8-24 h, the oxygen and carbon dioxide contents of all tested formulations could reach constant levels, in the ranges of 2-9% and 0-41%, respectively. These formulations were considered to be effective, safe, and easy to prepare and could be applied to wide varieties of food products.     

Application of Fourier transform midinfrared spectroscopy to the discrimination between Irish artisanal honey and such honey adulterated with various sugar syrups

A collection of authentic artisanal Irish honeys (n = 580) and certain of these honeys adulterated by fully inverted beet syrup (n = 280), high-fructose corn syrup (n = 160), partial invert cane syrup (n = 120), dextrose syrup (n = 160), and beet sucrose (n = 120) was assembled. All samples were adjusted to 70 degrees Bx and scanned in the midinfrared region (800-4000 cm(-1)) by attenuated total reflectance sample accessory. By use of soft independent modeling of class analogy (SIMCA) and partial least-squares (PLS) classification, authentic honey and honey adulterated by beet sucrose, dextrose syrups, and partial invert corn syrup could be identified with correct classification rates of 96.2%, 97.5%, 95.8%, and 91.7%, respectively. This combination of spectroscopic technique and chemometric methods was not able to unambiguously detect adulteration by high-fructose corn syrup or fully inverted beet syrup.     

Liquid chromatography coupled to isotope ratio mass spectrometry: a new perspective on honey adulteration detection

A new procedure to determine individual sugar (sucrose, glucose, and fructose) 13C isotope ratios, using liquid chromatography-isotope ratio mass spectrometry (HPLC-IRMS), has been developed to improve isotopic methods devoted to the study of honey authenticity. For this purpose 79 commercial honey samples from various origins were analyzed. Values of delta13Choney ranged from -14.2 to -27.2", and delta13Cprotein ranged from -23.6 to -26.9". A very strong correlation is observed between the individual sugar 13C ratios, which are altered in the event of sugar addition, even at low levels. The use of Deltadelta13C [fruct-glu], Deltadelta13C [fruct-suc], and Deltadelta13C [gluc-suc] systematic differences as an authenticity criterion permits the sugar addition [C3, beet sugar; or C4, cane sugar, cane syrup, isoglucose syrup, and high-fructose corn syrup (HFCS)] to be reliably detected (DL = 1-10%). The new procedure has advantages over existing methods in terms of analysis time and sensitivity. In addition, it is the first isotopic method developed that allows beet sugar addition detection.     

Detecting Corn Syrup in Barley Malt Extracts

Methods for detecting corn syrup in barley (Hordeum vulgare L.) malt extract were evaluated. Twelve samples representative of commercially available 2‐rowed and 6‐rowed malting barleys were malted. Extracts prepared from the finely ground malts were analyzed for ¹³C/¹²C ratios, expressed as δ¹³C, and concentrations of protein and sugars. The ¹³C/¹²C ratios were sufficiently different to distinguish corn syrup from malt extract. By calculating the mean values for the barleys, it was determined that a δ¹³C > ‐24.3‰ indicated that the malt extract had been adulterated with corn syrup (99% confidence). Protein concentrations <4.5% (2‐rowed malt) or <5.0% (6‐rowed malt) of the extracts also indicated probable adulteration with corn syrup, which is devoid of protein. Because of differences in sugar concentrations between the malt extracts and corn syrup, carbohydrate analysis also indicated probable mixtures. These findings were confirmed by analysis of extracts from composite 2‐rowed and 6‐rowed barley malts that had been mixed with known quantities of corn syrup. The regressions for δ¹³C, protein concentration, and most sugar concentrations against percent dilution with corn syrup in the mixtures were significant.     

Detection of sugar adulterants in apple juice using fourier transform infrared spectroscopy and chemometrics

Fourier transform infrared spectroscopy and attenuated total reflection sampling have been used to detect adulteration of single strength apple juice samples. The sample set comprised 224 authentic apple juices and 480 adulterated samples. Adulterants used included partially inverted cane syrup (PICS), beet sucrose (BS), high fructose corn syrup (HFCS), and a synthetic solution of fructose, glucose, and sucrose (FGS). Adulteration was carried out on individual apple juice samples at levels of 10, 20, 30, and 40% w/w. Spectral data were compressed by principal component analysis and analyzed using k-nearest neighbors and partial least squares regression techniques. Prediction results for the best classification models achieved an overall (authentic plus adulterated) correct classification rate of 96.5, 93.9, 92.2, and 82.4% for PICS, BS, HFCS, and FGS adulterants, respectively. This method shows promise as a rapid screening technique for the detection of a broad range of potential adulterants in apple juice.     

Improved Protocols for ELISA Determination of Gliadin in Glucose Syrups

Simple modifications of existing protocols for high‐sensitivity detection of gluten proteins by immunochemical methods allowed rapid and sensitive determination of residual gluten in highly viscous samples of glucose and maltose syrups obtained from processing wheat starch. Dilution of the original syrup to no less than 15–20% in solids allowed retention of gluten proteins in a soluble form so that ELISA determination of gliadin was possible without an extraction step in aqueous ethanol. An ultrafiltration step may be added to concentrate residual gluten proteins in the diluted syrup samples and allow a further increase in sensitivity. The results are relevant for quality assessment of wheat starch derived syrups as raw materials for use in gluten‐free foods for celiac individuals.     

Influence of strawberry yogurt composition on aroma release

The primary objective of this study was to determine how yogurt ingredients affect aroma release in the mouth during eating. A model strawberry flavor consisting of ethyl butanoate, ethyl 3-methylbutanoate, (Z)-hex-3-enol, 2-methylbutanoic acid, 5-hexylhydro-2(3H)-furanone, and 3-methyl-3-phenylglycidic acid ethyl ester was added to unflavored, unsweetened yogurt that had different added sweeteners and hydrocolloids. In all, 12 yogurt formulations were examined to determine the effects of gelatin, modified food starch, pectin, sucrose, high-fructose corn syrup, and aspartame on aroma release. Aroma release was monitored by breath-by-breath analysis (proton-transfer reaction-mass spectrometry) during eating of the test yogurts. Results showed aroma release of the ethyl butanoate, (Z)-hex-3-enol, and ethyl 3-methylbutanoate to be suppressed by sweeteners, with 55 DE high-fructose corn syrup having the greatest effect. Addition of thickening agents had no significant effect on the aroma release profiles of the compounds under study.     

Cell viability effects and antioxidant and antimicrobial activities of Tunisian date syrup (Rub El Tamer) polyphenolic extracts

The aqueous-acetone polyphenolic extract of the traditionally derived date syrup, known as "Rub El Tamer", was analyzed using RP-HPLC-DAD and ESI-MS. The phenolic content of the extract was 394.53 ± 1.13 mg per 100 g of syrup with caffeoylsinapylquinic acid as the most abundant compound (72.23%). The extract exhibited strong antioxidant activities as evaluated using the ABTS (2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid)), DPPH (2,2-diphenyl-1-picrylhydrazyl) and FRAP (ferric reducing antioxidant power) methods. The extract antimicrobial potential against a range of microorganism strains showed that Staphylococcus aureus, Staphylococcus epidermidis, and Bacillus cereus were the most sensitive bacteria with MBC in the range of 0.5-0.05 mg/mL. Furthermore, in the presence of the syrup extract (8.18-131 μg/mL), the Human SH-SY5Y neuroblastoma and the 3T3 fibroblast cell lines showed dissimilar reduction of viability suggesting a higher cytotoxic effect against tumorigenic cells. Our results provide new insights into date syrup characterization which should stimulate further studies of this hot desert resource.     

Use of differential scanning calorimetry (DSC) as a new technique for detection of adulteration in honeys. 1. Study of adulteration effect on honey thermal behavior.

Differential scanning calorimetry (DSC) was used to study the thermal behavior of authentic honeys (Lavandula, Robinia, and Fir honeys) and industrial sugar syrups. Thermal or thermochemical parameters such as the glass transition temperature (Tg), enthalpies of fusion (DeltaH(fus)), and heat capacity variation (DeltaC(p)) were measured. The syrups and honeys showed significant differences in thermal phenomena, as well as in their amplitude and position on the temperature scale. Results showed good reproducibility of the method for all samples studied. The effect of adulteration of honey with different amounts of syrup (5, 10, 20, 40, and 60%) was investigated. A linear relationship was found between the percentage of added syrup and the glass transition temperature. A similar relationship was obtained from the enthalpy of fusion results in the temperature range of 40-90 degrees C. Under applied conditions, the effects of adulteration of honeys by industrial syrups appeared to be detectable from a level as low as 5%.     

A new methodology based on GC-MS to detect honey adulteration with commercial syrups

Honey adulterations can be carried out by addition of inexpensive sugar syrups, such as high fructose corn syrup (HFCS) and inverted syrup (IS). Carbohydrate composition of 20 honey samples (16 nectar and 4 honeydew honeys) and 6 syrups has been studied by GC and GC-MS in order to detect differences between both sample groups. The presence of difructose anhydrides (DFAs) in these syrups is described for the first time in this paper; their proportions were dependent on the syrup type considered. As these compounds were not detected in any of the 20 honey samples analyzed, their presence in honey is proposed as a marker of adulteration. Detection of honey adulteration with HFCS and IS requires a previous enrichment step to remove major sugars (monosaccharides) and to preconcentrate DFAs. A new methodology based on yeast (Saccharomyces cerevisiae) treatment has been developed to allow the detection of DFAs in adulterated honeys in concentrations as low as 5% (w/w).     

Effect of Isomaltooligosaccharide Syrup on Quality Characteristics of Sponge Cake

Sponge cakes were formulated using isomaltooligosaccharide (IMO) syrup as a sweetener to replace 0, 25, 50, 75, and 100% sucrose. The qualities of cakes were evaluated by physicochemical, microbiological, and sensory evaluation analyses. The viscosity in cake batter, cake volume, crumb Hunter a value, and IMO contents of baked cakes increased with increasing IMO syrup level, whereas the specific gravity in cake batter, crust L a b, and crumb L and b values, and hardness of baked cakes showed a reverse trend. The crust and crumb of cakes became darker and less yellow and had a better tender and less sweet texture as IMO syrup level increased and sucrose decreased. The degree of overall liking of cakes increased with increasing IMO syrup level. Total plate counts exceeded 10⁵ CFU/g for cakes stored at 25°C for three days and <10³ CFU/g for the samples stored at 5°C for seven days. The changes in the moisture content, water activity, L a b values, and IMO contents of samples did not differ during storage. Overall, sucrose in the formulation of sponge cakes could be partially or fully replaced with IMO syrup.     

基于量纲分析的函数理论建立挤压脱胚玉米生产淀粉糖浆的糖化液过滤问题的经验公式

该文应用基于量纲分析的函数理论和蒋亦元修正的G.Murphy定理,扩大试验范围,减少试验次数,研究脱胚玉米挤压系统参数,对挤压脱胚玉米生产淀粉糖浆的糖化液滤速、DE值的影响规律。解决用脱胚玉米挤压膨化物生产淀粉糖浆难于糖化过滤的问题,为在实际生产中使用挤压膨化脱胚玉米生产淀粉糖浆提供参考。     

Thin layer chromatographic determination of deoxynivalenol in processed grain products

The thin layer chromatographic (TLC) method of Trucksess et al. (J. Assoc. Off. Anal. Chem. (1984) 67, 40-43) was modified for the determination of deoxynivalenol (DON) in high-sugar breakfast cereals, corn syrup, and beer. Celite was added to the substrate before extraction with acetonitrile-water (84 + 16). After filtration through an alumina-charcoal-Celite (0.5 + 0.7 + 0.3) column, the filtrate was evaporated to dryness and redissolved in water, which was passed through an octylsilyl reverse phase column. DON was eluted with anhydrous ethyl ether. The residue remaining after the eluate was evaporated to dryness was dissolved in CHCl3-acetonitrile (4 + 1) and chromatographed on AlCl3-impregnated silica gel TLC plates. The blue fluorescent DON spot was quantitated fluorodensitometrically after the TLC plate was heated at 120 degrees C for 7 min. Recoveries of DON added to breakfast cereals at 100, 200, and 400 ng/g levels and to syrup and beer at 50, 100, and 200 ng/g levels averaged 86%. The limit of determination in these products was about 50 ng/g.