首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献，搜索用时 33 毫秒
1.
A method for the quantitation of dityrosine in wheat flour and dough by high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) using an isotope dilution assay with the internal standard 3,3'-(13)C(2)-dityrosine in the single-reaction monitoring mode was developed. The method consisted of the release of protein-bound dityrosine by hydrolysis in 4 mol/L hydrochloric acid/8.9 mol/L propionic acid for 24 h at 110 degrees C after addition of the internal standard, cleanup by C(18) solid-phase extraction, and HPLC-MS/MS. The limit of detection of dityrosine was 80 ng/g of sample (0.22 nmol/g), and the limit of quantitation was 270 ng/g of sample (0.75 nmol/g). The method was sensitive enough to analyze wheat flour and dough and to study the effect of flour improvers on the dityrosine content. Furthermore, the effect of the mixing time was studied. The dityrosine concentration in the flour was 0.66 nmol/g. After we mixed a dough to peak consistency, the dityrosine concentration doubled and remained constant on further mixing. Overdoses of hydrogen peroxide and hexose oxidase (HOX, E.C. 1.1.3.5) resulted in a strongly increased dityrosine content, whereas no increase of the dityrosine concentration was found after the addition of ascorbic acid and potassium bromate. Calculation of the percentage of dimeric tyrosine showed that less than 0.1% of the tyrosine residues of wheat protein were cross-linked. Therefore, dityrosine residues seem to play only a very minor role in the structure of wheat gluten.  相似文献   

2.
A new gas chromatographic method is described for the analysis of fungicides captan, captafol, and folpet from organic extracts of air samples using large volume injection (LVI) via a cold on-column (COC) inlet coupled with gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). Although standard split/splitless injection due to high injection port temperatures (>225 degrees C) have been shown to degrade these thermally labile fungicides, COC injection minimizes degradation. Insecticides such as chlorpyrifos and diazinon were also examined to show added selectivity. By using a solvent vapor exit with the COC inlet, injection volumes of 10-100 microL can be made to lower detection levels. GC-NCI-MS was compared to GC-electron impact ionization-mass spectrometry for each pesticide using LVI-COC injections and was found to be 2-80 times more sensitive, depending on the pesticide. Method detection limit (MDL) values with 100 microL injections were 2.5 microg L-1 for captan, folpet, and diazinon, 5.0 microg L-1 captafol, and 1.0 microg L-1 for chlorpyrifos, with the normal working range examined for sample analysis from MDL to 100 microg L-1. Detection of all pesticides except captafol, used only in the United States but not Canada, was demonstrated from air samples taken from Abbotsford, British Columbia, Canada.  相似文献   

3.
The objective of this research was to compare the efficacy of potassium bromate with that of ozone treatment in wheat flour oxidation for breadmaking. In the first experiment, flour was treated with ozone at 1,500 ppm for 2, 4.5, 9, and 18 min. In the second experiment, flour was fully treated with ozone at 1,500 ppm for 45 min and then blended with control flour at concentrations of 10–30% (w/w). Flour became whiter and less yellow as ozonation time increased when compared to control flour. Size‐exclusion HPLC detected an increase in SDS buffer insoluble polymeric proteins in flour exposed to ozone. Bread made from flour treated with ozone for 2–4.5 min and bread that was made from flour blended with fully ozonated flour at 5 and 10% (w/w) was not significantly different for specific volume when compared with bread made with flour containing potassium bromate. Bread made from flour treated with ozone for 2, 4.5, and 9 min had a greater number of cells in crumb with larger loaf volumes than control flour. Results indicate that ozone treatment of flour could eliminate the need for potassium bromate in breadmaking.  相似文献   

4.
Benzothiazoles are a part of the molecular structure of a large number of natural products, biocides, drugs, food flavors, and industrial chemicals. They also appear in the environment mainly as a result of their production and use as rubber vulcanization accelerators. A new headspace solid-phase microextraction (HS-SPME) method for analysis of benzothiazole (BTH) in wine is described. This method is fast, inexpensive, and does not require solvents. The detection limit of BTH in wine was 45 ppt with linearity up to 100 ppb. The quantification of BTH is performed by the standard additions method and does not require the use of an internal standard. We have analyzed 12 wines from different grape varieties grown in several regions, using SPME extraction and gas chromatography-mass spectrometry (GC-MS) detection. Under these experimental conditions, benzothiazole was found in all wines analyzed. Concentration levels in samples varied from 0.24 microg/L (Vermentino) to 1.09 microg/L (Franciacorta).  相似文献   

5.
Among allergenic foods, soybean is known as a food causing adverse reactions in allergenic patients. To clarify the validity of labeling, the specific and sensitive detection method for the analysis of the soybean protein would be necessary. The p34 protein, originally characterized to be p34 as an oil-body associated protein in soybean, has been identified as one of the major allergenic proteins and named Gly m Bd 30K. A novel sandwich enzyme-linked immunosorbent assay (ELISA) for the detection and quantification of the soybean protein in processed foods was developed using polyclonal antibodies raised against p34 as a soybean marker protein and the specific extraction buffer for extract. The developed sandwich ELISA method was highly specific for the soybean protein. The limit of detection (LOD) and the limit of quantification (LOQ) of the developed ELISA were 0.47 ng/mL (equivalent to 0.19 microg/g in foods) and 0.94 ng/mL (equivalent to 0.38 microg/g in foods), respectively. The recovery ranged from 87.7 to 98.7%, whereas the intra- and interassay coefficients of variation were less than 4.2 and 7.5%, respectively. This study showed that the developed ELISA method is a specific, precise, and reliable tool for the quantitative analysis of the soybean protein in processed foods.  相似文献   

6.
A highly sensitive and rapid biosensor test based on disposable screen-printed thick-film electrodes was developed, which is suitable for monitoring organophosphate and carbamate residues in foods of animal origin with increased fat contents such as milk. The wild-type enzyme was combined with three engineered variants of Nippostrongylus brasiliensis acetylcholinesterase (NbAChE), to obtain enhanced sensitivity. The sample pretreatment could be reduced to a minimum. There was no extraction or fat removal necessary. With the biosensor test paraoxon concentrations down to 1 microg/L could be detected in milk. The detection limit for carbaryl was 20 microg/L. Recovery rates for paraoxon and carbaryl in milk samples lay between 89 and 107%. Ten milk samples from local markets were tested both with the biosensor test and with standard chromatographic multiresidue methods. Two milk samples caused AChE inhibition rates of >50%. Accordingly, 4 microg/L tebufenpyrad, 4 microg/L tetraconazole, and 2 microg/L bifenthrin were detected in one of these milk samples. The other milk sample contained 2 microg/L tebufenpyrad.  相似文献   

7.
Rugged LC-MS/MS survey analysis for acrylamide in foods   总被引：8，自引：0，他引：8  
The described liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the detection of acrylamide in food entails aqueous room temperature extraction, SPE cleanup, and analysis by LC-MS/MS. The method is applicable to a wide variety of foods. [(13)C(3)]acrylamide is the internal standard. The limit of quantitation is 10 ppb (microg/kg). Data were obtained in duplicate from >450 products representing >35 different food types. The variability in analyte levels in certain food types suggests that it may be possible to reduce acrylamide levels in those foods.  相似文献   

8.
An analytical multiresidue method for the simultaneous determination of various classes of pesticides in soil was developed. Pesticides were extracted from soil with ethyl acetate. Soil samples were placed in small columns, and the extraction was carried out assisted by sonication. Pesticides were determined by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. Pesticides were confirmed by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.2, 0.1, and 0.05 microg/g fortification levels of each pesticide, and the recoveries obtained ranged from 87.0 to 106.2% with a relative standard deviation between 2.4 and 10.6%. Good resolution of the pesticide mixture was achieved in approximately 41 min. The detection limits of the method ranged from 0.02 to 1.6 microg/kg for the different pesticides studied. The developed method is linear over the range assayed, 25-1000 microg/L, with determination coefficients >0.999. The proposed method was used to determine pesticide levels in real soil samples, taken from different agricultural areas of Spain, where several herbicides and insecticides were found.  相似文献   

9.
Due to its carcinogenicity and mutagenicity, furazolidone has been prohibited completely from being used in food animal production in the world since 1995. To monitor the illegal abuse of furazolidone, a polyclonal antibody-based indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) was developed for the determination of tissue-bound furazolidone metabolite 3-amino-2-oxazolidone (AOZ). The highly specific antibody was targeted for PAOZ, the benzaldehyde derivative of AOZ. The 50% inhibition values (IC 50) of 0.91 microg/L for AOZ was achieved with the most sensitive antibody Ab-B1 by altering ELISA conditions. In the ELISA, sample extraction and cleanup were performed by an is MAX cartridge following combined hydrolysis of the tissue-bound AOZ and derivatization of the homogenized tissues with benzaldehyde. The limits of detection (LOD) calculated from the analysis of 20 known negative tissue samples (swine liver, swine muscle, chicken liver, chicken muscle,and fish muscle) were 0.3-0.4 microg/kg (mean+3 SD). Recoveries of AOZ fortified at the levels of 0.4, 1, and 5 microg/kg ranged from 55.8 to 96.6% in the tissues. The coefficients of variation were less than 20% over the range of AOZ concentrations studied. The linear detection range was between 0.1 and 25.6 microg/L. Validation of the ELISA method with swine muscle and liver from furazolidone-treated pigs was carried out using HPLC, resulting in a similar correlation in swine muscle (r=0.99) and in swine liver (r=0.98). The results suggest that this ELISA is a specific, accurate, and sensitive method of detecting AOZ residues in animal edible tissues.  相似文献   

10.
A method was developed for the determination of the biocide ortho-phenylphenol (biphenyl-2-ol; OPP) in beer, using deuterated OPP as an internal standard. A new liquid-liquid extraction procedure, employing acetonitrile, diethyl ether, and n-pentane, afforded rapid phase separation. The evaporated extract was derivatized with pentafluorobenzyl bromide in a water-acetonitrile mixture that was buffered with potassium carbonate, followed by extraction of the derivative into cyclohexane and analysis by gas chromatography-mass spectrometry in electron ionization mode. The method enables the detection of OPP in 50 mL of beer at concentrations as low as 0.1 microg/L and provides a linear range of quantification of 0.5-40 microg/L. Samples from 61 beers canned over the past 12 years and sold in 27 countries were analyzed for OPP. In 40 of them, the target compound was present at concentrations of 1.2-40 microg/L. Our investigations indicate that the ends of the cans, which contain sealing material presumably treated with OPP, are responsible for this contamination.  相似文献   

11.
An analytical method has been developed for the quantification of two herbicides (ethidimuron and methabenzthiazuron) and their two main soil derivatives. This method involves fluidized-bed extraction (FBE) prior to cleanup and analysis by reverse-phase liquid chromatography with UV detection at 282 nm. FBE conditions were established to provide efficient extraction without degradation of the four analytes. (14)C-labeled compounds were used for the optimization of extraction and purification steps and for the determination of related efficiencies. Extraction was optimal using a fexIKA extractor operating at 110 degrees C for three cycles (total time = 95 min) with 75 g of soil and 150 mL of a 60:40 v/v acetone/water mixture. Extracts were further purified on a 500 mg silica SPE cartridge. Separation was performed on a C18 Purosphere column (250 mm x 4 mm i.d.), at 0.8 mL min(-1) and 30 degrees C with an elution gradient made up of phosphoric acid aqueous solution (pH 2.2) and acetonitrile. Calibration curves were found to be linear in the 0.5-50 mg L(-1) concentration range. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. Recovery values, determined from spiked samples, were close to 100%. Limits of detection ranged between 2 and 3 microg kg(-1) of dry soil and limits of quantification between 8 and 10 microg kg(-1) of dry soil. An attempt to improve these performances by using fluorescence detection following postcolumn derivatization by orthophthalaldehyde-mercaptoethanol reagent was unsuccessful.  相似文献   

12.
Eight methods were compared for the extraction of DNA from raw potato tubers, and nine methods were evaluated for the extraction of DNA from dehydrated potato slices, potato flakes, potato flour, potato starch, and two ready-to-eat potato snack foods. Extracts were assessed for yield using a fluorescence-based DNA quantification assay. Real-time amplification of an endogenous gene, sucrose synthase (sus), was used to assess extract and template quality. A CTAB-based method extracted the highest DNA yields from the tuber material. An in-house method, which utilized the Kingfisher magnetic particle processor, yielded the highest template quality from the tubers. For most of the tuber samples, the Kingfisher and CTAB methods recovered the highest levels of amplifiable sus. DNA yields for potato-derived foods generally decreased with the extent that the product had been processed. The methods that utilized the magnetic particle processor delivered the highest template quality from one of the snack products that was particularly high in fat. For most of the remaining processed products, the levels of amplifiable target DNA recovered were roughly correlated with total DNA recovery, indicating that overall yield had greater influence over sus amplification than template quality. The Wizard method was generally the best method for the extraction of DNA from most of the potato-derived foods.  相似文献   

13.
A simple, environmentally friendly, cost-effective, and sensitive method was developed for the determination of trace cadmium in rice by flow injection (FI) on-line precipitation preconcentration coupled with flame atomic absorption spectrometry (FAAS). The precipitation preconcentration of trace cadmium was achieved by on-line merging of the sample and ammonia solutions. The resultant precipitates were on-line collected by a knotted reactor (KR) without filtration. A solution of 1 mol L(-1) HNO(3) was employed to dissolve the collected precipitates and to deliver the analyte into the FAAS system for on-line detection. Preconcentration at a sample loading flow rate of 3.8 mL min(-1) for 35 s gave an enhancement factor of 44 and a detection limit (3sigma) of 0.002 microg g(-1) for the solid sample with a sample throughput of 72 h(-1). The precision (RSD, n = 11) was 2.0% at the 4.0 microg L(-1) level. The concentration of cadmium in a certified reference material (GBW 08511, rice flour) by the developed method using simple aqueous standards for calibration was in good agreement with the certified value. The proposed method was also successfully applied to the determination of trace cadmium in locally collected rice samples.  相似文献   

14.
A rapid LC-MS method, which compares different mass analyzers-single quadrupole, ion trap, and triple quadrupole-was developed for the quantitative determination of isopropyl thioxanthone (ITX) in fruit juices. ITX, a photoinitiator in UV-cured inks that can reach foods from the cartons for beverages in which they are used, was extracted from fruit juice samples with acetone/hexane (50:50) using pressurized liquid extraction. This method gave detection limits of 3, 3, and 0.01 microg/L and quantification limits of 10, 10, and 0.05 microg/L using single quadrupole, ion trap, and triple quadrupole, respectively. Five replicate fortifications of different fruit juices at the quantification limit gave recoveries oscillating between 68 and 72% with CV varying between 14 and 18%. This is the first report of a positive mass spectrometric identification and quantification of ITX in fruit juice samples packed in TetraPack. The sensitivity and specificity of the LC-MS/MS analysis using the triple quadrupole enables it to be the method of choice for risk assessment and monitoring. The method was applied to apricot, orange, peach, apple, grape and pineapple, and cherry and strawberry juices and to fruit nectars from Spain and Italy, and the ITX was detected in the range of 0.05-0.78 microg/L.  相似文献   

15.
An HPLC method has been developed for the analysis of extracts of fresh peppers containing capsaicinoids and of both capsaicinoids and piperines in pepper-containing foods produced and sold in Korea. The HPLC method was optimized by defining how composition of the mobile phase affected retention times. Both identification and quantification were based on retention times and the following criteria: linearity of the UV response at 280 nm in HPLC, recoveries from spiked samples, and observed individual molecular ions in the mass spectra of the extracts determined by liquid chromatography-mass spectrometry. This method, with a limit of detection of approximately 15-30 ng, was used to quantify the distribution of capsaicinoids in 11 Korean whole peppers and in 12 commercial pepper-containing foods. Total capsaicinoid levels of whole peppers ranged from 1.21 microg/g for the PR Gang ja variety to 121.1 microg/g for the Chung yang variety. The levels in food extracts, four of which also included two piperines, ranged from 11.0 microg/g for radish kimuchi to 3752 microg/g for capsaicin sauce. The results demonstrate (a) the usefulness of the HPLC method for the simultaneous analysis of capsaicinoids derived from red peppers and piperines derived from black and white peppers extracted from complex food matrices and (b) the wide-ranging spread of levels of pungent pepper compounds in fresh peppers and in pepper-containing foods consumed in Korea.  相似文献   

16.
Aflatoxins are a group of very carcinogenic mycotoxins that can be found on a wide range of food commodities including nuts, cereals, and spices. In this study, the first LC-MS/MS stable isotope dilution assay (SIDA) for the determination of aflatoxins in foods was developed. The development of this method was enabled by easily accessible isotope-labeled (deuterated) aflatoxins B2 and G2, which were synthesized by catalytic deuteration of aflatoxin B1 and G1, purified, and well-characterized by NMR and MS. All four aflatoxins of interest (B1, B2, G1, and G2) were quantified in food samples by using these two labeled internal standards. The response factors (RF) of the linear calibrations were revealed to be matrix independent for labeled aflatoxin B2/aflatoxin B2 and labeled aflatoxin G2/aflatoxin G2. For labeled aflatoxin B 2/aflatoxin B 1 and labeled aflatoxin B2/aflatoxin G1 matrix-matched calibration was performed for the model matrices almonds and wheat flour, showing significant differences of the RFs. Limits of detection (LOD) were determined by applying a statistical approach in the presence of the two model matrices, yielding 0.31 microg/kg (aflatoxin B1), 0.09 microg/kg (aflatoxin B2), 0.38 microg/kg (aflatoxin G1), and 0.32 microg/kg (aflatoxin G2) for almonds (similar LODs were obtained for wheat flour). Recovery rates were between 90 and 105% for all analytes. Coefficients of variation (CV) of 12% (aflatoxin B1), 3.6% (aflatoxin B2), 14% (aflatoxin G1), and 4.8% (aflatoxin G2) were obtained from interassay studies. For further validation, a NIST standard reference food sample was analyzed for aflatoxins B1 and B2. The method was successfully applied to determine trace levels of aflatoxins in diverse food matrices such as peanuts, nuts, grains, and spices. Aflatoxin contents in these samples ranged from about 0.5 to 6 microg/kg.  相似文献   

17.
A simple, rapid and sensitive multiresidue method has been developed for the determination in vegetables of organophosphorus pesticides commonly used in crop protection. Pesticide residues are extracted from samples with a small amount of ethyl acetate and anhydrous sodium sulfate. No additional concentration and cleanup steps are necessary. Analyses are performed by large volume GC injection using the through oven transfer adsorption desorption (TOTAD) interface. The calculated limits of detection for each pesticide injecting 50 microL of extract and using an NPD are lower than 0.35 microg/kg which is much lower than the maximum residues levels (MRLs) established by European legislation. Repeatability studies yielded a relative standard deviation lower than 10% in all cases. The method was applied to the analysis of eggplant, lettuce, pepper, cucumber, and tomato.  相似文献   

18.
A collaborative study was performed to validate the performance of the 1-2 TEST for detection of motile salmonellae in foods. Detection is based on observation of an immobilized band of cells. Twenty-three laboratories participated in the study. The 1-2 TEST (immunodiffusion test) was compared with the standard culture procedure (BAM/AOAC; FDA Bacteriological Analytical Manual) for detection of Salmonella in 6 food types: ground black pepper, soy flour, dried whole egg, milk chocolate, nonfat dry milk, and raw deboned turkey. Uninoculated and inoculated samples were included in each food group analyzed. After the tests on the 6 foods were completed, analysis of the data for turkey and soy flour showed that certain collaborators obtained data inconsistent with the data from the majority of collaborators. No specific method deviations to account for the inconsistencies were reported by those collaborators, so the collaborative testing of these 2 foods was repeated. Analysis of data for pepper, chocolate, nonfat dry milk, dried whole egg, and the second set of soy flour and turkey indicated 96.1% agreement between the BAM/AOAC and immunodiffusion test methods. The false negative rates for the immunodiffusion test and BAM/AOAC methods were 3.6 and 1.7%, respectively. There was no significant difference in the productivity of the immunodiffusion test and BAM/AOAC method at the 5% level for any of the 6 foods. The immunodiffusion screening method has been approved official first action for detection of motile Salmonella in foods.  相似文献   

19.
The maturation of Madeira wines usually involves exposure to relatively high temperatures and humidity levels >70%, which affect the aroma and flavor composition and lead to the formation of the typical and characteristic bouquet of these wines. To estimate the levels of sotolon [3-hydroxy-4,5-dimethyl-2(5H)-furanone] and their behavior over time, 86 aged Madeira wines samples (1-25 years old), with different sugar concentrations, respectively, 90 g L(-)(1) for Boal, 110 g L(-)(1) for Malvazia, 25 g L(-)(1) for Sercial, and 65 g L(-)(1) for Verdelho varieties, were analyzed. Isolation was performed by liquid-liquid extraction with dichloromethane followed by chromatographic analysis by GC-MS. The reproducibility of the method was found to be 4.9%. The detection and quantification limits were 1.2 and 2.0 microg L(-)(1), respectively. The levels of sotolon found ranged from not detected to 2000 microg L(-)(1) for wines between 1 and 25 years old. It was observed that during aging, the concentration of sotolon increased with time in a linear fashion (r = 0.917). The highest concentration of sotolon was found in wines with the highest residual sugar contents, considering the same time of storage. The results show that there is a strong correlation between sotolon and sugar derivatives: furfural, 5-methylfurfural, 5-hydroxymethylfurfural, and 5-ethoxymethylfurfural. These compounds are also well correlated with wine aging. These findings indicate that the kinetics of sotolon formation is closely related with residual sugar contents, suggesting that this molecule may come from a component like sugar.  相似文献   

20.
A collaborative study was performed in 11 laboratories to validate a DNA hybridization (DNAH) procedure for detection of Salmonella in foods. The DNAH procedure was compared to the standard culture method for detection of Salmonella in 6 foods: ground pepper, soy flour, dry whole egg, milk chocolate, nonfat dry milk, and raw deboned turkey. With the exception of turkey which was naturally contaminated, uninoculated and inoculated samples of each food group were analyzed. Results for the DNAH method were significantly better than for the standard culture method at the 5% probability level for the detection of Salmonella in turkey. There was no significant difference between the methods for the other 5 foods. The method has been adopted official first action.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号