Discrimination of Citrus reticulata Blanco and Citrus reticulata 'Chachi' as well as the Citrus reticulata 'Chachi' within different storage years using ultra high performance liquid chromatography quadrupole/time-of-flight mass spectrometry based metabolomics approach.

Using ultra high performance liquid chromatography quadrupole/time-of-flight mass spectrometry (UPLC-QTOFMS) based metabolomics, we focused on developing a method for the comprehensive distinction between Citri Reticulatae Blanco Pericarpium(CRBP) and Citri Reticulatae Chachi Pericarpium (CRCP), as well as the CRCP within different storage years in this study. Through this, we hope to enhance Citri Reticulatae Pericarpium (CRP) Quality Control system. Using UNIFI software and an online database identified chemical components in the 3-30 years CRCP(40 batches) and CRBP (10 batches)samples, and multivariate statistical analysis methods and heat-map were applied to distinguish between CRCP and CRBP and CRCP in different storage years. The results showed that a total of 92 compounds were identified from CRCP and CRBP samples, most of which were flavonoids. Principal component analysis (PCA) and orthogonal partial least squares discrimination analysis (OPLS-DA) indicated that it can effectively distinguish between CRBP and CRCP and various storage years CRCP, and 19 metabolites were identified as potential markers for distinguishing between CRBP and CRCP, and 15 potential markers showed a higher level of CRCP than CRBP. At the same time, 31 metabolites were identified to distinguish CRCP in different storage years, metabolite levels increased in 3-10 years and decreased after 15-30 years. Therefore, this approach can effectively distinguish between CRCP and CRBP and CRCP with different storage years, and may also provide a feasible strategy for the certification of Chinese herbal medicines from different species and storage years.

Identification of antioxidants in Fructus aurantii and its quality evaluation using a new on-line combination of analytical techniques.

A new on-line method for simultaneous identification and monitoring of antioxidants in Fructus aurantii was established by coupling high performance liquid chromatography-diode array detector-electrospray ionisation-ion trap-time of flight-mass spectrometry with post-column derivatisation and luminol-potassium ferricyanide chemiluminescence (HPLC-DAD-ESI-IT-TOF-MS-PCD-LPFCL). While the HPLC fingerprint, structural identification and radical scavenging profile were rapidly obtained by an on-line assay using ultraviolet (UV) absorption, MS and LPFCL, details of the precise substitution patterns of various structures were achieved through UV absorption using PCD addition of shift reagents. Twenty-five flavonoids were identified by either their PCD and MS data or comparison with reference substances. Data collected both from chromatograms and activity profiles of 12 samples revealed significant differences among samples from different habitats. The results showed that this method was rapid and precise, and therefore would be an effective and sensitive method for biocompounds analysis and quality evaluation for complex food and medicinal samples.

Requisitos de calidad de los aceites esenciales: importancia de las monografías de la Farmacopea Europea y de las normas ISO / Quality requirements for essential oils: importance of the monographs of the European Pharmacopoeia and ISO standards

Los aceites esenciales son productos naturales utilizados por diferentes industrias, entre las que destacan la alimentaria y la farmacéutica. Debido a la variabilidad inherente a los productos naturales y a los crecientes problemas de adulteraciones, el presente artículo tiene como objetivo promover y llamar la atención sobre la importancia de las normas internacionales existentes, especialmente las monografías de la Farmacopea Europea y las normas ISO, haciendo simultáneamente una comparación de los principales requisitos de estas directrices. Sólo el cumplimiento de estas normas puede garantizar que los aceites esenciales utilizados para diferentes fines tienen la calidad deseable para el propósito al que se destinan y que no se produzcan problemas de seguridad (AU)

Essential oils are natural products used by different industries, among which stand out pharmaceutical and food industries. Due to the variability inherent to all natural products and also to the growing problems of adulteration, this article aims to promote and draw attention to the importance of existing international standards, including the monographs of the European Pharmacopoeia and ISO standards, while making a comparison of the main requirements of these guidelines. Only the fulfillment of these standards can ensure that the essential oils used for different purposes have the desirable quality for the intended use and do not cause safety issues (AU)

Rapid simultaneous determination of amines and organic acids in citrus using high-performance liquid chromatography.

Rapid analytical method for the simultaneous separation and determination of amines and organic acids is a vital interest for quality control of citrus and their products. In the present study, a simultaneous high performance liquid chromatography (HPLC) method for the rapid separation of three amines and two organic acids was developed. Chromatographic separation of compounds was achieved using Xbridge C(18) column at ambient temperature, with an isocratic mobile phase of 3mM phosphoric acid at a flow rate of 1.0 mL min(-1). A photodiode array (PDA) detector was used to monitor the eluent at 223 nm and 254 nm with a total analysis time of 10 min. Extraction of amines and organic acids from citrus juice was optimized. The method was validated by tests of linearity, recovery, precision and ruggedness. The limit of detection (LOD) and limit of quantification (LOQ) for amines and ascorbic acid were determined to be 5 ng and 9.8 ng, respectively. All calibration curves showed good linearity (R(2) ≥ 0.9999) within the test ranges. The recoveries of the amines and organic acids ranged between 84% and 117%. The identity of each peak was confirmed by mass spectral (MS) analysis. The developed method was successfully applied to analyze the content of amines and organic acids in six different species and two varieties of citrus. Results indicate that mandarin and Marrs sweet orange contain high level of amines, while pummelo and Rio Red grapefruit had high content of ascorbic acid (137-251 µg mL(-1)) and citric acid (5-22 mg mL(-1)). Synephrine was the major amine present in Clementine (114 µg mL(-1)) and Marrs sweet orange (85 µg mL(-1)). To the best of our knowledge, this is the first report on simultaneous separation and quantification of amines and organic acids in Marrs sweet orange, Meyer lemon, Nova tangerine, Clementine, Ugli tangelo and Wekiwa tangelo.

Survival and development of immature stages of the Mediterranean fruit fly (Diptera: Tephritidae) in citrus fruit.

We studied, under laboratory conditions, the performance of the Mediterranean fruit fly, Ceratitis capitata (Wiedemann) (Diptera: Tephritidae), immature stages in intact whole fruit of three sweet orange varieties, lemon, and bitter oranges. Both citrus variety and fruit part (flavedo, albedo, and pulp) had strong effects on larval performance, smaller effects on pupae, and no effects on eggs. Fruit peel was the most critical parameter for larval development and survival, drastically affecting larval survival (inducing very high mortality rates). Among fruit regions, survival of larvae placed in flavedo was zero for all varieties tested except for bitter orange (22.5% survival), whereas survival in albedo was very low (9.8-17.4%) for all varieties except for bitter orange (76%). Survival of pupae obtained from larvae placed in the above-mentioned fruit regions was high for all varieties tested (81.1-90.7%). Fruit pulp of all citrus fruit tested was favorable for larval development. The highest survival was observed on bitter oranges, but the shortest developmental times and heaviest pupae were obtained from orange cultivars. Pulp chemical properties, such as soluble solid contents, acidity, and pH had rather small effects on larval and pupal survival and developmental time (except for juice pH on larvae developmental duration), but they had significant effects on pupal weight.

Certification of standard reference materials containing bitter orange.

A suite of three dietary supplement standard reference materials (SRMs) containing bitter orange has been developed, and the levels of five alkaloids and caffeine have been measured by multiple analytical methods. Synephrine, octopamine, tyramine, N-methyltyramine, hordenine, total alkaloids, and caffeine were determined by as many as six analytical methods, with measurements performed at the National Institute of Standards and Technology and at two collaborating laboratories. The methods offer substantial independence, with two types of extractions, two separation methods, and four detection methods. Excellent agreement was obtained among the measurements, with data reproducibility for most methods and analytes better than 5% relative standard deviation. The bitter-orange-containing dietary supplement SRMs are intended primarily for use as measurement controls and for use in the development and validation of analytical methods.

Genotype and harvest time influence the phytochemical quality of Fino lemon juice (Citrus limon (L.) Burm. F.) for industrial use.

Two clonal selections of lemon tree (Citrus limon Burm. f. cv. Fino), named Fino-49-5 and Fino-95, were studied to ascertain the influence of genetic (clone) and environmental (season) factors on the human-health bioactive compounds of lemon juice (vitamin C and flavonoids) and the possible relationship between composition and in vitro antioxidant capacity (2,2-diphenyl-1-picrylhydrazyl, 2,2'-azino-bis(3-ethyl-benzothiazoline-6-sulfonic acid), and ferric reducing antioxidant power) of the juice. The cultivar Fino-49-5 performed better in terms of flavonoid and vitamin C contents. Variability in the weather conditions determined, at least in part, differences in the content of lemon juice bioactives more importantly than the genetic background did. Therefore, the food industry would have phytochemically rich and nutritive lemons with practically complete independence of the harvest time and the selected cultivar.

Storage temperature effects on blood orange fruit quality.

Orange fruits of two blood varieties (Tarocco and Moro) were stored at 8 degrees C and 22 degrees C for 85 and 106 days, respectively, and analyzed periodically for standard quality parameters (total soluble solids, total acidity, ascorbic acid, juice yield, and rind color) and sensory influencing parameters (anthocyanins, and total and free hydroxycinnamic acids). A decrease in total acidity (TA) and juice yield during storage was observed for both cultivars; total soluble solids (TSS) increased only in the Tarocco oranges stored at 8 degrees C. The increase in TSS observed for Tarocco and the simultaneous decrease in TA in both varieties resulted in a higher maturity index (TSS/TA) for the two cultivars. No loss of vitamin C was noted in Tarocco orange at either temperature, whereas a sharp reduction in vitamin C occurred in the first 50 days of storage for Moro. A significant increase in anthocyanin content was observed in Tarocco and Moro stored at 8 degrees C. Overlong storage induces extensive hydrolysis of hydroxycinnamic derivatives to free acids in Moro orange and these, in turn, could develop the malodorous vinylphenols.

Microwave-assisted extraction method for the determination of atrazine and four organophosphorus pesticides in oranges by gas chromatography (GC).

A simple and rapid microwave assisted extraction (MAE) method is presented for the determination of atrazine and four organophosphorus pesticides (parathionmethyl, chlorpyriphos, fenamiphos and methidathion) in orange peel. The experimental variables that affect the MAE method, such as temperature, sample quantity, extraction time, nature and volume of organic solvents, were optimized. The MAE method was optimized using an experimental design. The results suggest that temperature and sample quantity are statistically significant factors. It was concluded that the five pesticides could be efficiently extracted from 1.5-2.5 g of orange peel with 10 mL of hexane/acetone (1: 1) mixture at 90 degrees C in 9 min with microwave power set at 50% (475 W). After optimization these factors, recoveries ranged from 93 to 101% with a relative standard deviation ranging from 1 to 3%. The extracts were analyzed by gas chromatography with a nitrogen-phosphorus detector (GC-NPD).

Differentiation of several geographical origins in single-strength Valencia orange juices using quantitative comparison of carotenoid profiles.

Pure Valencia orange (Citrus sinensis) juices (64 samples) from Spain, Israel, Belize, Cuba, and Florida, harvested during two seasons (1996-1997 and 1997-1998), were analyzed for their carotenoid profiles. The detection of saponified carotenoid pigments has been achieved and quantitated using a photodiode array detection monitored at 350, 430, and 486 nm. Carotenoid pigments commonly found in the orange variety Valencia have been separated on a polymeric C-30 column using a ternary gradient as eluent. Pure Valencia juices from oranges grown in Mediterranean regions (Israel and Spain) have a high carotenoid content, expressed in beta-carotene (5-18 and 14-35 mg L(-)(1), respectively), compared to those grown in tropical and subtropical regions (Cuba, Belize, and Florida) (4-10, 2-8, and 5-10 mg L(-)(1), respectively). Quantitative results allowed the differentiation of Valencia variety geographical origins, in particular, the Mediterranean area from tropical and subtropical areas, using multidimensional analyses of carotenoid contents.

Differentiation of several geographical origins in single strength Valencia orange juices using quantitative comparison of carotenoid profiles

Pure Valencia orange (Citrus sinensis) juices (64 samples) from Spain, Israel, Belize, Cuba, and Florida, harvested during two seasons (1996-1997 and 1997-1998), were analyzed for their carotenoid profiles. The detection of saponified carotenoid pigments has been achieved and quantified using a photodiode array detection monitored at 350, 430, and 486 nm. Carotenoid pigments commonly found in the orange variety Valencia have been separated on a polymeric C-30 column using a ternary gradient as eluent. Pure Valencia juices from oranges grown in the Mediterranean regions (Israel and Spain) have a high carotenoid content, expressed in beta-carotene (5-18 and 14-35 mg L(-)(1), respectively), compared to those grown in tropical and subtropical regions (Cuba, Belize, and Florida) (4-10, 2-8, and 5-10 mg L(-)(1), respectively). Quantitative results allowed the differentiation of Valencia variety geographical origins, in particular, the Mediterranean area from tropical and subtropical areas, using multidimensinal analyses of carotenoid contents. (AU)

Effects of energy source and food flavor on conditioned preferences in sheep.

Livestock and range managers would have a powerful tool to direct utilization and modify plant communities if animals could be conditioned to eat specific foods or plants. We attempted to condition preferences for a low-quality forage through nutrient loading. Sheep were fed licorice or orange-flavored straw pellets then were gavaged with glucose or propionate (.381 Mcal, which amounted to approximately 13% of the daily maintenance energy requirement) or water. Four groups of ewes (n = 4) were arranged in a cross-blocked design such that each group received a unique energy/flavor combination: 1) propionate+licorice, 2) propionate+orange, 3) glucose+licorice, or 4) glucose+orange. On alternate days, each group received the other flavor plus water to create an internal control. At the end of 8 d of conditioning, preference for the two flavors was measured by two-choice preference tests. A second trial was conducted for 4 d in which the energy level was doubled to .762 Mcal. Low energy levels of either glucose or propionate did not create significant preferences. Propionate at the low-level caused satiety but at the high level conditioned an aversion to both flavors. This high level of propionate apparently caused malaise that was then associated with the taste of the flavors. The high level of glucose conditioned a preference. The high glucose treatment increased rumen microbial mass, the nutrients of which would have been absorbed in the lower gastrointestinal tract, and may have indirectly provided the positive nutrient feedback required to form a preference. There was a flavor preference for orange that was independent of the energy supplements.

Determination of optimum pH and temperature for pasteurization of citrus juices by response surface methodology.

Optimization of microbial death, enzyme inactivation and vitamin C retention during pasteurization of pH-adjusted orange juice is discussed free of equipment-dependent parameters such as the heating lag. The pH-temperature optimum was determined by response surface methodology in the range of 65 degrees C-75 degrees C and pH 2.5-4.0. The results implied that there was no pectinesterase activity below pH 3.5. Leuconostoc mesenteroides had its maximum and minimum thermal resistance at pH 3.5 and pH 2.7, respectively. For an ideal theoretical process requiring four log cycles of microbial reduction the optimum pasteurization conditions were 12 min at 75 degrees C and pH 2.7.

[Studies on the preparation and evaluation of Kijitsu, the immature citrus fruits. III. Relation between diameter of Kijitsu and synephrine content].

For the purpose of evaluating Kijitsu, the content of synephrine in dried unripe citrus fruits was analyzed by high performance liquid chromatography after cleaning up the MeOH extract with an ion exchange cellulose column. Among them, Citrus unshiu had the highest amount of synephrine. No difference was found between C. hassaku and C. aurantium. The synephrine content decreased corresponding with an increase in diameter of Kijitsu.

Citrus fruits--varieties, chemistry, technology, and quality evaluation. Part II. Chemistry, technology, and quality evaluation. A. Chemistry.

In Part 2 of this review on citrus fruits, the literature on chemistry, technology, and quality evaluation are critically considered. Sweet oranges, mandarin, grapefruit, lemon, and lime are generally used for processing. The literature on chemical components of citrus fruit which include sugars, polysaccharides, oraganic acids, nitrogenous constituents and lipids; carotenoids which contribute to color; vitamins and minerals, and flavonoids; limonoids, some of which impart bitterness to the juice; and the volatile components which contribute to aroma have been reviewed. Chilled and pasteurized juices, juice concentrates, and beverages are the important products manufactured commercially, and to a limited extent powdered citrus juices, canned segments, and marmalades. The literature on the manufacture of these products also as new types of juice and oil extractors; TASTE and other types of evaporators; tank farms to store juice and concentrate in bulk; aseptic filling in bulk containers and retail packs; alternate flexible and rigid containers other than glass and tin; and recovery of volatile flavoring constituents during juice processing are some of the important technological developments in the recent past and have been discussed. Bitterness in citrus juices and its control, composition of cloud, and its stability and changes during storage have been reviewed. Essential oils, pectin, frozen and dried juice sacs, dried pulp and molasses, flavonoids, seed oil, and meal are the important byproducts, the manufacture of which is given in essential details. Generally, consumers judge the product on the basis of its sensory attributes. The quality of finished product is dependent upon the raw materials used and control of processes. The U.S. Department of Agriculture (USDA) standards for different products, physicochemical and microbiological parameters prescribed as indices of quality of fruit, juice, concentrate, and other products; composition of essential oils; and aroma concentrates are discussed in relation to sensory quality. Analytical methods for compounds affecting quality, and methods for detection of adulteration in different citrus products are briefly reviewed. The importance of sensorily evaluating quality of citrus products to select and develop quality control indices is emphasized. Areas where further research are required are indicated. A comprehensive bibliography is provided to aid further study and research.

Citrus fruits. Part II. Chemistry, technology, and quality evaluation. B. Technology.

In Part II of this review on citrus fruits, the literature on chemistry, technology, and quality evaluation are critically considered. Sweet oranges, mandarin, grapefruit, lemon, and lime are generally used for processing. The literature on chemical components of citrus fruit which include sugars, polysaccharides, organic acids, nitrogenous constituents and lipids; carotenoids which contribute to color; vitamins and minerals and flavonoids; limonoids, some of which impart bitterness to the juice; and the volatile components which contribute to aroma were reviewed in section A. Chilled and pasteurized juices, juice concentrates, and beverages are the important products manufactured commercially, and to a limited extent powdered citrus juices, canned segments, and marmalades. The literature on the manufacture of these products also as new types of juice and oil extractors; TASTE and other types of evaporators; tank farms to store juice and concentrate in bulk; aseptic filling in bulk containers and retail packs; alternate flexible and rigid containers other than glass and tin; and recovery of volatile flavoring constituents during juice processing are some of the important technological developments in the recent past and have been discussed in this section. Bitterness in citrus juices and its control, composition of cloud, and its stability and changes during storage have been reviewed. Essential oils, pectin, frozen and dried juice sacs, dried pulp and molasses, flavonoids, seed oil, and meal are the important byproducts, the manufacture of which is given in essential details. Generally, consumers judge the product on the basis of its sensory attributes. The quality of finished product is dependent upon the raw materials used and control of processes. In section C, the U.S. Department of Agriculture (USDA) standards for different products, physicochemical and microbiological parameters prescribed as indices of quality of fruit, juice, concentrate, and other products; composition of essential oils; and aroma concentrates are discussed in relation to sensory quality. Analytical methods for compounds affecting quality, and methods for detection of adulteration in different citrus products are briefly reviewed. The importance of sensorily evaluating quality of citrus products to select and develop quality control indices is emphasized. Areas where further research are required are indicated. A comprehensive bibliography is provided to aid further study and research.

[Study and identification of adulteration of citrus fruit juices]. / Recherche et identification de quelques adultérations dans le jus d'agrumes.

UNLABELLED: Various types of adulterations. Definition and method of determination. Case of fraud by standardization. Definition and problems. Specific problems of these types of frauds. Qualitative definition. 1. Automatic methods of classification: --ascending hierarchical classification; --analysis of correspondances; --analysis of "composantes principales". 2. RESULTS: Classification of juices according to the main types of fraud (watering, sugaring, acidification, comminuted intensification). 3. Towards a quantitative solution. Conclusion. Interest of the method, possibilities and limits, further possible uses.

Orange juice quality with an emphasis on flavor components.

This review studies the chemistry of the flavor of citrus juices with emphasis on the components of the flavor of orange juice and their origin in the different parts of the orange fruit. Citrus processing and the nature of the various products as they affect flavor are discussed. The composition of peel oil, aroma oil, orange juice, orange essence, and orange essence oil is presented. The relationship between flavor and color are discussed and the role of lipid components as they affect flavor stability and off-flavors are described. Spoilage resulting from microbes is briefly treated. The nutritional value of orange juice is cited.

Stability of ascorbic acid in orange juice exposed to light and air during storage.

Single-strength orange juice prepared from three nationally available brands of frozen orange juice concentrate was analyzed for ascorbic acid after exposure to light and air for varying periods up to eighteen days. For two of the brands, brown, foil-covered bottles offered no greater protection against ascorbic acid loss than clear glass bottles. Storage time appeared to be a greater contributor to ascorbic acid loss than type of container in two brands. One brand showed both the effect of storage time and type of container, since the juice stored in the brown bottle lost significantly less ascorbic acid after the same period than juice stored in the clear bottle.