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1.
Heated plant foods may contain compounds with adverse health effects (e.g. acrylamide). On the other hand, health-promoting compounds (e.g. antioxidants) have also been identified in such foods. Therefore, a baking experiment with biscuits was carried out to study the potential impact of both acrylamide and antioxidants in that food. Two different wheat flour types - wholemeal (WMF) and white flour type 550 (T550; 0.55% mineral content) - as well as recipe (fat and leavening agent) and thermal input (temperature?×?time) were changed. Furthermore, the effect of an enzymatic asparagine hydrolysation was tested. Antioxidants were determined with two independent procedures ABTS - (2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonate)) and FRAP-assay (ferric reducing ability of plasma). WMF samples resulted in an unchanged acrylamide level, but in a significantly higher antioxidant concentration when compared with T550 samples (149 and 141?μg?kg(-1) acrylamide and 9.1 and 5.1?mmol?TE?kg(-1) FW ABTS for WMF and T550, respectively). A reduced fat content yielded in an increased volume. Raising agents had no effect on acrylamide levels, but antioxidants were higher in samples with sodium bicarbonate (SBC) than with ammonium bicarbonate (ABC). Thermal input (temperature?×?time; 150°C?×?25?min to 240°C?×?9?min) indicated an exponential acrylamide increase especially at higher temperatures (from 75 to 236?μg?kg(-1)), whereas antioxidant increase was linear (from 7.0 to 7.7?mmol?TE?kg(-1) FW, ABTS). FRAP and ABTS values were correlated on a low level, whereas acrylamide content of biscuits was correlated with FRAP and lightness (R (2?)=?0.62 and 0.47, and 0.71 and 0.85 for WMF and T550, respectively). The enzyme asparaginase reduced acrylamide formation by about 50% for both raising agents (SBC and ABC, respectively), whereas antioxidant levels were not affected. An evaluation of recipe variants with low acrylamide and high antioxidants indicated the advantage of wholemeal biscuits.  相似文献   

2.
A deterministic exposure assessment using the Nusser method that adjusts for within-subject variation and for nuisance effects among Finnish children and adults was carried out. The food consumption data covered 2038 adults (25–74 years old) and 1514 children of 1, 3 and 6 years of age, with the data on foods’ acrylamide content obtained from published Finnish studies. We found that acrylamide exposure was highest among the 3-year-old children (median?=?1.01?µg?kg?1?bw?day?1, 97.5th percentile?=?1.95?µg?kg?1?bw?day?1) and lowest among 65–74-year-old women (median?=?0.31?µg?kg?1?bw?day?1, 97.5th percentile?=?0.69?µg?kg?1?bw?day?1). Among adults, the most important source of acrylamide exposure was coffee, followed by casseroles rich in starch, then rye bread. Among children, the most important sources were casseroles rich in starch and then biscuits and, finally, chips and other fried potatoes. Replacing lightly roasted coffee with dark-roasted, swapping sweet wheat buns for biscuits, and decreasing the acrylamide content of starch-based casseroles and rye bread by 50% would result in a 50% decrease in acrylamide exposure in adults. Among children, substituting boiled potatoes for chips and other friend potatoes and replacing biscuits with sweet wheat buns while lowering the acrylamide content of starch-based casseroles by 50% would lead to acrylamide exposure that is only half of the original exposure. In conclusions, dietary modifications could have a large impact in decreasing acrylamide exposure.  相似文献   

3.
BACKGROUND: Strawberries are nutritive fruits and a source of antioxidants. We evaluated antioxidant properties of ‘Camino Real’ strawberries grown in the Brazilian savannah, harvested in different seasons. Analytical and meteorological data were analyzed by partial least squares regression. RESULTS: Fruits from May showed the lowest contents of total phenolics (1789.78 mg kg?1 fresh weight (FW)), catechin (21.37 mg kg?1 FW), quercetins (4.89 mg kg?1 FW) and total ellagic acid (208.68 mg kg?1 FW) and the lowest antioxidant activity by 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) (11.39 mg Butylated hydroxytoluene (BHT) eq. g?1 FW) and ferric reducing antioxidant power (FRAP) (22.01 mg ferrous sulfate eq. g?1 FW) assays. Strawberries harvested in July presented the lowest concentrations of total (190.61 mg kg?1 FW) and individual anthocyanins (73.88 mg kg?1 FW and 5.96 mg kg?1 FW for pelargonidin‐3‐glucoside and cyanidin‐3‐glucoside, respectively), but the highest contents of vitamin C (685.47 mg kg?1 FW), DPPH (18.87 mg BHT eq. g?1 FW) and FRAP (39.30 mg ferrous sulfate eq. g?1 FW). The highest contents of free ellagic acid (26.11 mg kg?1 FW), pelargonidin‐3‐glucoside (291.82 mg kg?1 FW) and cyanidin‐3‐glucoside (11.84 mg kg?1 FW) were found in strawberries from September. Rain in the previous 30 days to harvest influenced negatively many phenolics and antioxidant activity of strawberries harvested in May. In July, longer photoperiod and lower temperature at 30 days previous to harvest probably led to higher antioxidant activity and vitamin C. Increased photoperiod and temperature at the final stage of maturation seem to raise pigments and free ellagic acid in strawberries. CONCLUSION: It was possible to observe significant relationships among meteorological and antioxidant variables for strawberries grown in the Brazilian savannah. Copyright © 2011 Society of Chemical Industry  相似文献   

4.
The main by‐product from the table olive canning industry is the stone with some residual olive flesh. The purpose of this study was to evaluate the composition – phenolic compounds (hydroxytyrosol, tyrosol and oleuropein) and tocopherol – and the antioxidant activity in different fractions (flesh, stone and seed) from the table olive by‐product and the whole by‐product. The highest amounts of phenolic compounds (1710.0 ± 33.8 mg kg?1) as well as the highest antioxidant activity (8226.9 ± 9.9 hydroxytyrosol equivalents mg kg?1) were obtained in the seed. The highest amounts of hydroxytyrosol (854.8 ± 66.0 mg kg?1) and tyrosol (423.6 ± 56.9 mg kg?1) were found in the whole by‐product from the pepper stuffed olives, while the stone without seed had the maximum oleuropein content (750.2 ± 85.3 mg kg?1). α‐Tocopherol values were between 79.8 ± 20.8 mg kg?1 in the seed of the olive stone and 6.2 ± 1.2 mg kg?1 in the whole by‐product from the anchovy‐stuffed olives. In light of the results obtained, it would seem possible to use table olive by‐product as a source of natural antioxidants in foods, cosmetics or pharmaceutical products, thus contributing to diminishing the environmental impact of table olive by‐product and to its revalorisation.  相似文献   

5.
This study investigated the organic acid and phenolic compound levels, total phenolic (TP) and antioxidant capacity (TEAC) of three miniature tomato cultivars grown on a farmer’s field with three different fertilizer applications. Analysis of phenolic compound (protocatechuic, vanillic, gallic, chlorogenic, caffeic, syringic, p-coumaric and ferulic acid, rutin, quercetin, catechin and phloridzine) organic acid (citric, tartaric, malic, succinic and fumaric acid), TP and TEAC levels in fruit samples showed statistically significant (p?<?0.05) differences between tomato cultivars and fertilizer applications. Rutin and chlorogenic acid were the predominant phenolic compounds found in all three cultivars. The highest rutin value (50.48 mg kg?1 FW) was found in the Black Zebra fertilized with DAP plus organic and biochemical fertilizers and the lowest (20.52 mg kg?1 FW) in the Black Zebra fertilized with DAP only. The highest chlorogenic acid value (63.31 mg kg?1 FW) was found in the sweet pea currant fertilized with DAP only and the lowest (21.06 mg kg?1 FW) in the Black Zebra fertilized with DAP plus chemical fertilizer. Citric acid content was the dominant organic acid in all three cultivars, with the highest citric acid value (6439.50 mg kg?1 FW) found in the Sweet Pea Currant cherry tomato fertilized with DAP plus organic and biochemical fertilizers and the lowest (2435.20 mg kg?1 FW) in the Window Box Yellow fertilized with DAP plus chemical fertilizer. Total phenolic and antioxidant levels in the window box yellow were significantly lower as compared to the Black Zebra and sweet pea currant varieties for all three fertilizer applications.  相似文献   

6.
BACKGROUND: Apricot is one of the most popular Prunus species grown in the temperate zone and great variation in the contents of primary and secondary metabolites has been reported in its fruit. However, little is known on the phenolic profiles and antioxidant potential of important local cultivars. The objective of the study was to identify valuable parental lines for breeding of cultivars with high health‐promoting effects. RESULTS: Primary metabolites (sugars, organic acids) and secondary metabolites (phenolics) were quantified by high‐performance liquid chromatography–mass spectrometry (HPLC/MS) in fruit of 13 apricot cultivars: total sugars ranged from 59.2 to 212.5 g kg?1 fresh weight (FW) and total organic acids from 4.2 to 20.8 g kg?1 FW. Four hydroxycinnamic acids and three flavonols were quantified; their content was significantly higher in skin compared to pulp. Similarly, antioxidative potential was significantly higher in skin and ranged from 125.4 to 726.5 mg ascorbic acid equivalents kg?1 FW. A positive correlation between total phenolic content and antioxidant potential was determined. Multivariate analysis subdivided the cultivars into five major groups, mostly influenced by the content of individual and total phenolics as well as the antioxidant potential of apricot skin and pulp. CONCLUSION: In regard to high phenolic content in connection with antioxidant potential, three cultivars stand out as the richest in analyzed quality parameters: ‘Mula Sadik’, ‘Bergeron’ and ‘Chuan Zhi Hong’. They also contained high amounts of primary metabolites and should be promoted for further planting and included in apricot breeding programs. Copyright © 2010 Society of Chemical Industry  相似文献   

7.
ABSTRACT

The determination of acrylamide in potato products, bakery products and coffee, and the human dietary exposure is reported. The method reported is based on a single extraction step with water, followed by the clean-up of the extract using solid phase extraction columns and finally, the determination of acrylamide using UPLC–MS/MS. The MS/MS detection was carried out using an ESI interface in positive ion mode. Internal calibration was used for the quantification of acrylamide, because of the suppression/enhancement matrix effects due to the complex nature of the samples. The method performance characteristics were determined after spiking blank samples. The mean recoveries in spiked coffee samples, potato chips, breakfast cereals and crispbread ranged from 93% to 99%, with RSDs lower than 5% for both repeatability and reproducibility conditions. The estimated limits of detection and quantification of the method were 10 and 32 μg kg?1, respectively. The method was used for monitoring acrylamide in 406 samples. Acrylamide amounts ranged from <32 to 2450 μg kg?1. A total of 360 samples (89%) were contaminated with acrylamide, but only 14% of the samples exceeded the benchmark levels of the EU legislation. Foods with the highest mean acrylamide amounts were potato crisps (642 μg kg?1), French fries (383 μg kg?1) and biscuits (353 μg kg?1). The mean and 95th percentile acrylamide exposures of adolescents in Cyprus were 0.8 and 1.8 μg kg?1 body weight per day, respectively. The estimated levels of dietary exposure to acrylamide are not of concern with respect to neurotoxicity. However, the margins of exposure (MOEs) indicate a concern for carcinogenicity. Potato fried products (45%), fine bakery ware (21%) and potato chips (14%) contributed the most to overall acrylamide exposure.  相似文献   

8.
This research was undertaken to evaluate the sugars, organic acids, phenolic compositions and antioxidant capacities of sweet cherry cultivars (Van, Noir de Guben, Larian and 0‐900 Ziraat) grown in Turkey. High‐performance liquid chromatographic methods were used to identify and quantify four sugars (sucrose, glucose, fructose and sorbitol) and four organic acids (malic, citric, shikimic, and fumaric acid). The major organic acid was found as malic acid (8.54–10.02 g kg?1 of FW). With regard to sugars, glucose was present in the largest amounts (44.71–48.31 g kg?1 of FW) for sweet cherry cultivars. The sum of sugars ranged from 103.87 (Larian) to 113.13 g kg?1 of FW (0‐900 Ziraat) and that of organic acids from 12.01 (0‐900 Ziraat) to 14.17 g kg?1 of FW (Noir de Guben). A total of eleven phenolic compounds were identified and quantified in sweet cherry cultivars, including hydroxycinnamic acids (3), anthocyanins (5), flavan‐3‐ols (2) and flavonol (1) compounds. Total phenolic contents ranged from 88.72 (Van) to 239.54 (Noir de Guben) mg/100 g of FW, while antioxidant activities ranged from 2.02 to 7.75 μm Trolox equivalents g?1 of FW.  相似文献   

9.
A novel GC–MS method was developed for the determination of acrylamide, which is applicable to a variety of processed foods, including potato snacks, corn snacks, biscuits, instant noodles, coffee, soy sauces and miso (fermented soy bean paste). The method involves the derivatization of acrylamide with xanthydrol instead of a bromine compound. Isotopically labelled acrylamide (d 3-acrylamide) was used as the internal standard. The aqueous extract from samples was purified using Sep-Pak? C18 and Sep-Pak? AC-2 columns. For amino acid-rich samples, such as miso or soy sauce, an Extrelut? column was used for purification or extraction. After reaction with xanthydrol, the resultant N-xanthyl acrylamide was determined by GC–MS. The method was validated for various food matrices and showed good linearity, precision and trueness. The limit of detection and limit of quantification ranged 0.5–5 and 5–20?µg?kg?1, respectively. The developed method was applied as an exploratory survey of acrylamide in Japanese foods and the method was shown to be applicable for all samples tested.  相似文献   

10.
A simple, low-cost, sensitive and selective method for the determination of trace quantities of nitrite in foods such as cheese and cured meat using diffuse ultraviolet-visible reflectance was developed. It is based on the reaction of nitrite with sulphadiazine and α-naphthol, which produces a coloured product in basic medium. The reaction is carried out directly in the measuring cell. For cheese the limit of detection (LOD), expressed as NaNO2, was estimated to be about 2.0?×?10?2?mg?l?1 (2.9?×?10?7?mol?l?1) in the final measuring solution and 0.17?mg?kg?1 in cheese (2.5?×?10?6?mol?kg?1). The relative standard deviation (RSD) varied from 5% to 8% depending on the sample. For meat the LOD was estimated to be about 2.0?×?10?2?mg?l?1 (2.9?×?10?7?mol?l?1) in the final measuring solution and 0.13?mg?kg?1 in meat (1.9?×?10?6?mol?kg?1). The RSD varied from 3% to 6% depending on the sample. The results of the proposed method were also compared with those obtained with the official method using the statistical Student's t-test and F-test procedures.  相似文献   

11.
Nine commercial varieties of tomato (Rambo, Senior, Ramillete, Liso, Pera, Canario, Durina, Daniella and Remate) produced in Spain were analysed for their lycopene content, content of phenolic compounds and antioxidant capacity. The phenolic compounds were characterised as flavonoids (quercetin, kaempferol and naringenin) and hydroxycinnamic acids (caffeic, chlorogenic, ferulic and p‐coumaric acids). Antioxidant activity was measured using the DPPH and ABTS assays. The concentrations of lycopene and the various phenolic compounds as well as the antioxidant activity were significantly influenced by the tomato variety. Quercetin, the most abundant flavonoid, was found in concentrations ranging between 7.19 and 43.59 mg kg?1 fresh weight, while naringenin levels were lower than 12.55 mg kg?1. The most abundant hydroxycinnamic acid was chlorogenic acid, with values ranging from 14 to 32 mg kg?1 fresh weight, followed by caffeic acid, while p‐coumaric and ferulic acids showed similar concentrations lower than 5 mg kg?1. The highest content of lycopene was found in Ramillete, Pera and Durina (>50 mg kg?1 fresh weight), while the concentration in the other varieties was between 50 and 30 mg kg?1, with the exception of Liso (less than 20 mg kg?1). The antioxidant activity of tomato extracts varied with the tomato variety and the assay method used. Individual compounds found to be significantly related to antioxidant capacity were lycopene and ferulic and caffeic acids, but not quercetin and chlorogenic acid. © 2002 Society of Chemical Industry  相似文献   

12.
To evaluate the potential public health risk of ethyl carbamate (EC), EC exposure from fermented foods and beverages for Hong Kong population was estimated. In 276 samples analysed, EC was detected (limit of detection (LOD) at 0.4?µg?kg?1) in 202 samples (73%), with higher levels in fermented red bean curd (150–650?µg?kg?1) and yellow wine (140–390?µg?kg?1), while low or non-detected (ND) in preserved vegetables (ND–10?µg?kg?1) and fermented tea (ND–15?µg?kg?1). The estimated dietary exposure from all fermented foods and beverages was 8.27?ng?kg?1?bw?day?1, while exposure excluding alcoholic beverages was 5.42?ng?kg?1?bw?day?1, with calculated margins of exposure (MOEs) at 3.6?×?104 and 5.5?×?104 respectively. The risk of adverse health effects was low for the average population but higher (MOE?of?103) for high consumers of alcoholic beverages especially habitual drinkers of alcoholic types with high EC contents.  相似文献   

13.
Low-density polyethylene (LDPE)/polypropylene (PP) blend films in various blending ratios containing 3000?mg?kg?1 of tocopherol were manufactured by an extrusion process. Tocopherol release properties were characterised and correlated with antioxidant effectiveness in retarding the oxidation of linoleic acid contacting the films at 40°C. The conditions without tocopherol (control) and with instant tocopherol addition corresponding to the amount included in the films were also prepared and compared with the film-contacting solutions. The effect of tocopherol inclusion and the blending ratio on their physical properties was also examined. A wide range of tocopherol diffusivity in 6.6?×?10?16–4.6?×?10?14?m2?s?1 were obtained by blend films. As PP content increases, the diffusivity decreased sharply at the beginning and levelled off later. The slower release of tocopherol in LDPE/PP blend films corresponding to lower tocopherol diffusivity retained the higher tocopherol concentration in the linoleic acid system providing better antioxidant effectiveness of the extended induction period in oxidation. The tocopherol inclusion reduced tensile strength and transparency significantly in an affordable range with higher tensile strength given by a higher PP ratio. LDPE/PP blending can be a useful tool to modulate the release profile of tocopherol and thus the antioxidant effectiveness of the tocopherol-incorporated antioxidant packaging film.  相似文献   

14.
Acrylamide in Thai-conventional snacks was analysed by GC/MS with a linear response ranged of 5–50?µg and r 2?>?0.99. The limit of detection (s/n?=?(3) and limit of quantification (s/n?=?10) were 4 and 15?µg?kg?1, respectively, and RSD?<?2%. Acrylamide in 19 food samples ranged from <15?µg?kg?1 to 1.26?mg?kg?1 with highest concentrations in Kanom Jak. Moderate levels (150–500?µg?kg?1) were detected mostly in deep-fried products, especially sweet potato and taro crisps, Kanom Kai Hong, banana fritters, durian chips and spring rolls. Thai-conventional snacks possessed low concentrations (<150?µg?kg?1) including Khao Larm, Pa Tong Koo, sweet banana crisps and deep-fried Chinese wonton. Acrylamide was lowest (<15?µg?kg?1) in fish strips, rice crackers, Hoi Jor and fried fish balls. Dietary habits by 400 tourists indicate a daily intake of acrylamide <150?ng, well below a toxic dose.  相似文献   

15.
Potato crisps are one of the food commodities that contribute most to overall dietary human exposure of acrylamide. This investigation has estimated the dietary exposure to acrylamide form potato crisps in the Spanish population. Sampling of potato crisps (n = 36) from 16 different producers were carried out in March 2008. An average level of 740 µg kg?1 (ranging from 81 to 2622 µg kg?1; minimum to maximum) and a median of 592 µg kg?1 were obtained. Acrylamide levels in marketed potato crisps have been significantly reduced (nearly to 50%) compared with a previous sampling performed 4 years earlier. The observed signal value (90th percentile) was 1377 µg kg?1 with 86% of the samples with acrylamide levels lower than 1000 µg kg?1. Dietary exposure to acrylamide from potato crisp consumption in the total Spanish population was estimated to be 0.042 µg kg?1 body weight day?1 by using a deterministic approach based on the National consumption database. In a second study, dietary exposure (based on a 3-day food record) was determined to be 0.053 µg kg?1 body weight day?1 for the adult population (17–60 years) and 0.142 µg kg?1 body weight day?1 for children (7–12 years). The contribution of potato crisps to the estimated dietary acrylamide exposure of the Spanish population is moderate as compared with other European Member States.  相似文献   

16.
Selected sugars, organic acids and phenolic compounds were analysed in mature fruits of ‘Williams’ pears using high‐performance liquid chromatography. Fruits were harvested from the branches of trees tested in three treatments: branches were bent in summer 2003 (1 September), in spring 2004 (15 May) and control (branches were not bent). Pears contained up to 73.54 g kg?1 fresh weight (FW) of fructose, 9.42 g kg?1 FW of glucose, 7.94 g kg?1 FW of sucrose and 24.59 g kg?1 FW of sorbitol. Major organic acids were (in order of descending quantity) citric, malic, shikimic and fumaric acid (up to 3.05 g kg?1 FW, 2.24 g kg?1 FW, 71.79 mg kg?1 FW and 0.49 mg kg?1 FW, respectively). Chlorogenic acid (280.86–357.34 mg kg?1 FW) was the predominant phenolic acid, followed in concentration (mg kg?1 FW) by syringic acid (95.46–131.32), epicatechin (46.55–83.09), catechin (25.67–44.81), vanillic acid (1.87–3.48), sinapic acid (0.83–1.72) and caffeic acid (0.72–1.04). Significant differences in content of fructose, sorbitol, total sugars, catechin, epicatechin, sinapic acid, syringic acid, and a sum of determined phenolic compounds were observed among the treatments. Fruits from summer bending branches had the lowest content of individual sugars, citric acid and phenolic compounds and the highest content of malic, shikimic and fumaric acid. The highest content of fructose, sorbitol, sucrose, total sugars, caffeic acid, catechin, epicatechin and syringic acid were determined in the fruits from the spring treatment. In the control treatment the highest content of glucose, citric acid, chlorogenic acid, sinapic acid, vanillic acid, as well a sum of determined phenolics, were observed. The lowest content of fumaric acid was in the spring treatment and of malic and shikimic acid in the control. Copyright © 2006 Society of Chemical Industry  相似文献   

17.
The aim of the study was to investigate the interactions between selenium (Se) and various trace elements, both toxic and essential, involved in the antioxidant system. A total of 128?day-old chicks (Gallus gallus, broilers) were used to investigate the effect of Se yeast supplementation on the accumulation of cadmium (Cd), copper (Cu) iron (Fe) and zinc (Zn). There were four replicates of four dietary treatments: T1 (basal diet with no added Se, analyzed to contain 0.21?mg?kg?1), T2 (T1 with 0.15?mg?kg?1 Se added), T3 (T1 with 0.3?mg?kg?1 Se) and T4 (T1 with 3.0?mg?kg?1 Se). At week 4 and 6, two chickens per replicate pen were sacrificed for whole blood, breast muscle and liver sampling. Samples were analyzed by ICP–MS. Supplementation with Se-yeast, not only increased Se concentration but also reduced Cd concentration in the tissues. Selenium was negatively correlated with Cd and positively correlated with Zn, Cu and Fe. Cadmium was negatively correlated with Zn and Cu. Zinc was positively correlated with Cu. Iron was negatively correlated with Cu and uncorrelated with Zn and Cd. The balance between Se, Cu, Fe and Zn is important for proper antioxidant defense since they are an integral part of various antioxidant enzymes.  相似文献   

18.
BACKGROUND: Three new artichoke seed‐propagated hybrids (Tempo, Opal and Madrigal) were compared with two standard cultivated varietal types [Catanese and Violet du Provence (VP)] in terms of head morphology, processing performance, nutritional or technological qualitative traits, in order to define their best use. RESULTS: Compared to the other genotypes, Opal and Madrigal had more rounded, heavier, larger heads, higher processing yield (>400 g of heart kg?1 raw head) and lower total phenol (TP) content (2.4 g of gallic acid equivalents kg?1 FW). VP gave a higher processing yield than Catanese and showed the highest TP content (6.5 g kg?1 FW). Tempo hearts were more similar to those of VP in biometrical and chemical terms (P, Na, K, Ca); they had the highest dry matter content (163 g kg?1 FW) and the waste left after peeling had the highest TP content. CONCLUSIONS: Hybrid artichokes, especially Opal and Madrigal, appear more suitable for the processing industry and also for fresh‐cut production due to their highest processing yield and lowest total phenol content. Because of its high total phenol content, Tempo waste represents a possible source of natural antioxidant in the pharmaceutical field and in the food industry (as a food additive). Copyright © 2010 Society of Chemical Industry  相似文献   

19.
An efficient LC method was developed for screening the presence of quinolones (QLs) – comprising fluoroquinolones (FQs) and acidic quinolones (AQs) – residues in various livestock and fishery products. Targeted analytes were for nine FQs of marbofloxacin (MAR), ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR), danofloxacin (DAN), orbifloxacin (ORB), difloxacin (DIF) and sarafloxacin (SAR), and three AQs of oxolinic acid (OXA), nalidixic acid (NAL) and flumequine (FMQ). Samples comprised ten different food products covering five matrices: muscle (cattle, swine and chicken), liver (chicken), raw fish (shrimp and salmon), egg (chicken), and processed food (ham, sausage and fish sausage). This method involved a simple extraction with (1:1) acetonitrile–methanol, a highly selective clean-up with an immobilised metal chelate affinity column charged with Fe3+, a fast isocratic LC analysis using a short column (20?mm?×?4.6?mm, 3?µm) with a mobile phase of (15:85:0.1) methanol/water/formic acid, and fluorescence detection (excitation/emission wavelengths of 295?nm/455?nm for FQs (495?nm for MAR), and 320?nm/365?nm for AQs). Among FQs, pairs of NOR/OFL, ORB/DIF and ENR/DAN were incompletely resolved. A confirmatory LC run with a Mg2+ containing methanolic mobile phase was also proposed for the samples suspected of being positive. The optimised method gave satisfactory recoveries of 88.5% (56.1–108.6%) and 78.7% (44.1–99.5%) for intra- and inter-day assays with relative standard deviations of 7.2% (0.7–18.4%) and 6.8% (1.4–16.6%), respectively. Limits of quantitation ranged from 0.8?µg?kg?1 (DAN) to 6.5?µg?kg?1 (SAR). This method was successfully employed to analyse 113 real samples and two positive samples were found: fish sausage (CIP 990?µg?kg?1) and shrimp (ENR 20?µg?kg?1).  相似文献   

20.
Two microbiological kits based on Bacillus stearothermophilus (Eclipse 50® and Premi®Test) have been evaluated and validated according to the European guideline for the validation of screening methods (January 2010) and in relation to the concentrations recommended by the EU-RL in 2007. Both tests are robust, a fast method and easy to implement. Both tests are applicable to a very large variety of honeys from different floral and geographical origins (rosemary, lavender, scrub, heath, alder, forest, lemon, acacia, chestnut, raspberry, mountain and flowers) as well as honey of different colours (from blank honey to brown honey, including yellow and orange honey). A satisfactory false-positive rate of 5% was obtained for the Eclipse 50® test. The observed detection capabilities CCβ of the Eclipse 50® kit were: chlortetracycline (>75?µg?kg?1), oxytetracycline (≤200?µg?kg?1), tetracycline (>100?µg?kg?1), cloxacillin (≤40?µg?kg?1), tylosin (≤200?µg?kg?1), desmycosin (>400?µg?kg?1), sulfadiazine (≤300?µg?kg?1), sulfadimethoxine (≤250?µg?kg?1), sulfamerazine (>300?µg?kg?1), sulfamethazine (>1000?µg?kg?1), sulfamethizole (>75?µg?kg?1), sulfamethoxazole (≤25?µg?kg?1), sulfanilamide (?1000?µg?kg?1), sulfaquinoxaline (>75?µg?kg?1), sulfathiazole (≤250?µg?kg?1) and lincomycin (>1500?µg?kg?1). These levels were all higher than the recommended concentrations where they exist. Due to its lack of sensitivity, it cannot be recommended for reliable routine use. The observed CCβ of the Premi®Test kit were: chlortetracycline (10?µg?kg?1), oxytetracycline (>10?µg?kg?1), tetracycline (≤10?µg?kg?1), cloxacillin (≤5?µg?kg?1), tylosin (≤10?µg?kg?1), desmycosin (≤15?µg?kg?1), sulfadiazine (≤25?µg?kg?1), sulfadimethoxine (≤25?µg?kg?1), sulfamerazine (≤25?µg?kg?1), sulfamethazine (≤25?µg?kg?1), sulfamethizole (≤25?µg?kg?1), sulfamethoxazole (≤10?µg?kg?1), sulfanilamide (≤25?µg?kg?1), sulfaquinoxaline (≤10?µg?kg?1), sulfathiazole (25?µg?kg?1) and lincomycin (≤25?µg?kg?1). The Premi®Test kit could be recommended for reliable use in routine control due to its low detection capabilities (except for aminoglycosides), but the disadvantage is a high false-positive rate of 14%.  相似文献   

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