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1.
An assessment of the stability of a large number (106) of pesticides and related compounds during the cryogenic sample processing of apples has been undertaken. For the first time the procedure included an assessment of the losses during the freezing of the fruits, prior to processing. The stability of each pesticide during processing was assessed by comparing the mean recovery for the laboratory-spiked samples with the mean "survival" of the pesticides in cryogenically processed samples. The results clearly demonstrate that the vast majority, 94 of 106, of pesticides were stable during cryogenic processing. Of particular importance was that losses of several pesticides [bitertanol (95%), heptenophos (50%), isofephos (40%), and tolylfluanid (48%)] reported to occur during ambient processing of apples did not occur during cryogenic processing. Losses of dichlofluanid (54%), chlozolinate (22%), and etridiazole (40%), previously reported to occur during ambient processing of apples, were reduced to barely significant levels (10, 17, and 14%, respectively) by cryogenic processing. Small apparent losses for a few of the compounds were attributable to analytical and sample handling difficulties, rather than to losses during processing, and need further investigation.  相似文献   

2.
Residue levels of pyrifenox, pyridaben, and tralomethrin were determined in unprocessed and processed tomatoes, grown in a experimental greenhouse, to evaluate the effect of three different household processes (washing, peeling, and cooking) and the "unit to unit" variability of these pesticides in tomatoes. The study was carried out on 11 greenhouse tomato samples collected during a 5 week period in which two successive treatments with the studied pesticides were applied. Residue levels in unprocessed and processed tomato samples were determined by means of ethyl acetate extraction and gas chromatography-electron capture detection determination. The washing processing factor results were 0.9 +/- 0.3 for pyridaben, 1.1 +/- 0.3 for pyrifenox, and 1.2 +/- 0.5 for tralomethrin, whereas the peeling processing factors were 0.3 +/- 0.2 for pyridaben and 0.0 +/- 0.0 for both pyrifenox and tralomethrin. The average loss of water in the tomato pure samples during the cooking process was approximately 50%; the cooking processing factors were 2.1 +/- 0.8 for pyridaben, 3.0 +/- 1.1 for pyrifenox, and 1.9 +/- 0.8 for tralomethrin. The unit-to-unit variability factors were determined on three different greenhouse samples analyzing 10 different units of unprocessed tomatoes from each sample. In all cases, the unit-to-unit variability factor results were within the range of 1.3-2.2.  相似文献   

3.
A specific indicator of freshness, allowing routine distinction between freshly squeezed orange juices (FSOJs) and FSOJ-like products, was to be identified. Using the Actijoule unit of a tubular heater at a flow rate of 60 L/h, FSOJs from Citrus sinensis (L.) Osbeck cv. Valencia Late were continuously heated on a pilot plant scale at six different temperatures (42-92 degrees C), followed by continuous cooling to ambient temperature and subsequent filling into sterilized glass jars. The cloud stability and residual activities of pectin methylesterase (PE) and peroxidase (POD) were monitored over the storage at 4 degrees C for up to 62 days, thus considering the storage conditions of FSOJs in retail markets. As shown by the viable microbial counts throughout storage, microbial activity was insignificant due to good sanitary practice, thus proving that the enzyme activities detected were of plant origin. The juices processed at temperatures > or =62 degrees C were characterized by minor residual activities. When exposed to temperatures <62 degrees C in the genuine acidic matrix of the juices, the heat stability of PE exceeded that of POD. Compared with the aforementioned samples, the juice processed at 52 degrees C with a residual PE activity of 33.8% was hardly inferior in terms of cloud stability within the first 14 days. After the juice was processed at 42 degrees C, rapid clarification occurred within the first 8 days, consistent with undetectable PE deactivation. Hence, only the range of approximately 50-60 degrees C is relevant in minimal heat-processing for the retention of cloud stability within the short turnover period of FSOJ-like products, with partial PE and POD deactivation being already sufficient to distinguish those juices from FSOJs. Irrespective of the previous thermal treatment, the total PE activity remained nearly constant during storage, whereas the POD activity rapidly declined to minor levels after 20 days. Consequently, as to the future analysis of samples with unknown processing history, PE was suggested as an indicator enzyme for the freshness of FSOJs, allowing their unambiguous distinction from minimally heat-processed juices.  相似文献   

4.
A gel permeation chromatographic (GPC) method, used by the U.S. Environmental Protection Agency (USEPA), was modified for cleanup of soil, sediments, wastes, and oily wastes before determination of semivolatile organic pollutants. The modifications included new calibration procedures and control of the amount of material processed. The modifications were evaluated for soil and sediment matrixes in a 5-laboratory study where each laboratory processed a solution containing a phthalate, substituted phenols and benzenes, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), nitroaniline, and pesticides. With the exception of nitroaniline, analyte recoveries were 87-112%, with relative standard deviations (RSDs) of 6.7-26%. Soil samples containing PCBs and fortified with 6 pesticides at 0.7-4 micrograms/g were also analyzed by the 5 laboratories. The mean recovery of the 6 pesticides was 100% with a mean RSD of 16%. Mean RSD for the determination of total PCBs was 8.9%. An additional modification for the processing of wastes and high concentration waste samples was attempted; this involved GPC processing of sample extracts dissolved in 1 + 1 butyl chloride-methylene chloride. This modification did not improve recoveries of the semivolatile analytes. Finally, the modified GPC protocol was applied to PCB-contaminated reclaimed waste oils samples. Two GPC cleanup steps were used to separate PCBs from the waste oil samples before PCBs were determined by gas chromatography combined with electron-capture detection (GC/ECD).  相似文献   

5.
Soy isoflavones are widely recognized for their potential health benefits. The increased use of traditional and new food products calls for the assessment of their stability during processing and storage. The present study examines the stability of genistein and daidzein derivatives in soy milk. Soy milk was stored at ambient and elevated temperatures, and the change in isoflavone concentration was monitored with time. Genistin loss in time showed typical first-order kinetics, with rate constants ranging from 0.437-3.871 to 61-109 days(-1) in the temperature ranges of 15-37 and 70-90 degrees C, respectively. The temperature dependence of genistin loss followed the Arrhenius relation with activation energies of 7.2 kcal/mol at ambient temperatures and 17.6 kcal/mol at elevated temperatures. At early stages of soy milk storage at 80 and 90 degrees C, the 6' '-O-acetyldaidzin concentration increased, followed by a slow decrease. The results obtained in this study can serve as a basis for estimating the shelf life of soy milk as related to its genistin content.  相似文献   

6.
This study presents new sample preparation and analytical procedures for the quantification of pesticides on processed tea leaves. The new method includes tea extraction and dispersive solid phase extraction (d-SPE) to prepare gas chromatography (GC) and ultrahigh-performance liquid chromatography (UHPLC)-ready samples, providing a fast and cost-effective solution for time-sensitive industrial analysis to fulfill regulatory requirements. Both GC-negative chemical ionization mass spectrometry (GC-NCI-MS) and UHPLC-tandem mass spectrometry (UHPLC-MS/MS) were employed to produce highly sensitive and reproducible data. Excellent limits of detection (typically below 1 μg/kg for GC and 10 μg/kg for UHPLC), wide linearity ranges, and good recoveries (mostly >70%) were achieved on the selected pesticides. Twenty-seven tea samples purchased from local grocery stores were analyzed using the newly developed methods. Among the pesticides analyzed, endosulfan sulfate and kelthane were the most frequently detected by GC-NCI-MS and imidacloprid and acetamiprid by UHPLC-MS/MS in these teas. The samples were found to be relatively clean, with <1 mg/kg of total pesticide residues. The organic-labeled teas were significantly cleaner than nonorganic ones. The cost per gram of tea did not correlate with pesticide residue levels detected.  相似文献   

7.
Separate experiments by the U.S. Geological Survey (USGS) and the Illinois State Water Survey Central Analytical Laboratory (CAL) independently assessed the stability of hydrogen ion and specific conductance in filtered wet-deposition samples stored at ambient temperatures. The USGS experiment represented a test of sample stability under a diverse range of conditions, whereas the CAL experiment was a controlled test of sample stability. In the experiment by the USGS, a statistically significant (α=0.05) relation between [H+] and time was found for the composited filtered, natural, wet-deposition solution when all reported values are included in the analysis. However, if two outlying pH values most likely representing measurement error are excluded from the analysis, the change in [H+] over time was not statistically significant. In the experiment by the CAL, randomly selected samples were reanalyzed between July 1984 and February 1991. The original analysis and reanalysis pairs revealed that [H+] differences, although very small, were statistically different from zero, whereas specific-conductance differences were not. Nevertheless, the results of the CAL reanalysis project indicate there appears to be no consistent, chemically significant degradation in sample integrity with regard to [H+] and specific conductance while samples are stored at room temperature at the CAL. Based on the results of the CAL and USGS studies, short-term (45–60 day) stability of [H+] and specific conductance in natural filtered wet-deposition samples that are shipped and stored unchilled at ambient temperatures was satisfactory.  相似文献   

8.
Microwave-assisted extraction (MAE) was carried out for the simultaneous determination of the insecticides thiamethoxam [(EZ)-3-(2-chloro-1,3-thiazol-5-ylmethyl)-5-methyl-1,3,5-oxadiazinan-4-ylidene(nitro)amine], imidacloprid [1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine], and the fungicide carbendazim (methyl benzimidazol-2-ylcarbamate) in vegetable samples. Five crop samples consisting of cabbage, tomatoes, chilies, potatoes, and peppers were fortified with the three pesticides and subjected to MAE followed by cleanup to remove coextractives prior to analysis by high-performance liquid chromatography. Using the selected microwave exposure time and power setting, the recoveries of the three pesticides from the fortified vegetable samples ranged from 68.1 to 106%. The corresponding recoveries for samples processed simultaneously but without microwave exposure ranged from 37.2 to 61.4%. The recoveries by MAE were comparable to those obtained by the conventional blender extraction technique. The precision of the MAE method was demonstrated by relative standard deviations of <7% for the three pesticides. The cooked cabbage and tomato samples showed no breakdown of the parent compounds, and the recoveries of three pesticides were comparable to those obtained with the uncooked samples.  相似文献   

9.
Processed fruits and vegetables have been long considered to have lower nutritional value than their fresh commodities due to the loss of vitamin C during processing. This research group found vitamin C in apples contributed < 0.4% of total antioxidant activity, indicating most of the activity comes from the natural combination of phytochemicals. This suggests that processed fruits and vegetables may retain their antioxidant activity despite the loss of vitamin C. Here it is shown that thermal processing elevated total antioxidant activity and bioaccessible lycopene content in tomatoes and produced no significant changes in the total phenolics and total flavonoids content, although loss of vitamin C was observed. The raw tomato had 0.76 +/- 0.03 micromol of vitamin C/g of tomato. After 2, 15, and 30 min of heating at 88 degrees C, the vitamin C content significantly dropped to 0.68 +/- 0.02, 0.64 +/- 0.01, and 0.54 +/- 0.02 micromol of vitamin C/g of tomato, respectively (p < 0.01). The raw tomato had 2.01 +/- 0.04 mg of trans-lycopene/g of tomato. After 2, 15, and 30 min of heating at 88 degrees C, the trans-lycopene content had increased to 3.11+/- 0.04, 5.45 +/- 0.02, and 5.32 +/- 0.05 mg of trans-lycopene/g of tomato (p < 0.01). The antioxidant activity of raw tomatoes was 4.13 +/- 0.36 micromol of vitamin C equiv/g of tomato. With heat treatment at 88 degrees C for 2, 15, and 30 min, the total antioxidant activity significantly increased to 5.29 +/- 0.26, 5.53 +/- 0.24, and 6.70 +/- 0.25 micromol of vitamin C equiv/g of tomato, respectively (p < 0.01). There were no significant changes in either total phenolics or total flavonoids. These findings indicate thermal processing enhanced the nutritional value of tomatoes by increasing the bioaccessible lycopene content and total antioxidant activity and are against the notion that processed fruits and vegetables have lower nutritional value than fresh produce. This information may have a significant impact on consumers' food selection by increasing their consumption of fruits and vegetables to reduce the risks of chronic diseases.  相似文献   

10.
A method for the determination of organochlorine pesticides in soil samples combining microwave assisted micellar extraction (MAME) with solid-phase microextraction (SPME) and high-performance liquid chromatography-UV has been developed. A mixture of two nonionic surfactants (polyoxyethylene 10 lauryl ether and polyoxyethylene 10 stearyl ether) was used for the extraction of pesticides from agricultural soils, and different types of SPME fibers were compared. The different parameters which affect extraction efficiency in the SPME procedure were optimized such as extraction time and temperature. The method developed involves extraction and preconcentration for the target analytes in soil samples. The analytical parameters were also studied and good recoveries obtained, RSD being lower than 10% and detection limits ranging between 36 and 164 ng g(-1) for the pesticides studied. The proposed method was successfully applied to the determination of some organochlorine pesticides in several kinds of agricultural soil samples with different characteristics.  相似文献   

11.
Low-temperature blanching of vegetables activates the enzyme pectin methylesterase (PME), which demethylates cell wall pectins and improves tissue firmness. This temperature activation of PME has been investigated by measuring the formation of methanol in intact tissue of green beans and tomatoes. Rates of methanol formation at temperatures of 35-65 degrees C were obtained by measuring the release of methanol from thin slices of tomato pericarp or green bean pod material. Activation energies of 112 and 97 kJ mol(-1) were calculated for PME activity in green beans and tomatoes, respectively. These activation energies indicate that the rate of pectin demethylation at 65 degrees C will be nearly 100 times that at 25 degrees C. PME activity was also determined titrimetrically using a solubilized form of the enzyme and purified pectin at temperatures from 30 to 60 degrees C. Under these conditions, much lower activation energies of 37 and 35 kJ mol(-1) were obtained for green beans and tomatoes, respectively. Methanol accumulation during heating of whole intact green beans was also determined and yielded an activation energy similar to that obtained with sliced beans. Whole green beans held at room temperature did not accumulate any methanol, but sliced or homogenized beans did. If whole beans were first heated to 45 degrees C and then cooled, methanol accumulation was observed at room temperature. These results indicate that two factors contribute to the observed high rate of pectin de-esterification during low-temperature blanching: (1) An irreversible change, causing PME to become active, occurs by heating to > or = 45 degrees C. (2) The high activation energy for pectin de-esterification means that the rate of de-esterification increases substantially with increasing temperature.  相似文献   

12.
The analytical process of lycopene extraction and photometrical determination was critically examined for raw tomato and processed tomato products by means of a 2 IV (15-10) Plackett-Burman experimental design in order to identify the key factors (KFs) involved. Fifteen apparent key factors (AKFs) reported in the literature were selected: sample weight (X1); volume of extraction solution (X2); antioxidant concentration (BHT, X3); neutralizing agent concentration (MgCO 3, X4); light presence during lycopene extraction (X5), homogenization velocity (X6) and time (X7), agitation time (X8), and temperature (X9) during the extraction process; water volume for separation of polar/nonpolar phases (X11); presence of inert atmosphere throughout the process (X12); time (X13), temperature (X14), and light presence (X10) during separation of phases and time delay for reading (X15). In general, higher lycopene concentrations in samples led to a higher number of key factors (KF). Thus, for raw tomato (lycopene range 1.22-2.29 mg/100 g) no KF were found, whereas for tomato sauce (lycopene range from 5.80 to 8.60 mg/100 g) one KF (X4) and for tomato paste (lycopene range from 35.80 to 51.27 mg/100 g) five KFs (X1, X2, X4, X11, and X12) were detected. For lycopene paste, X1 and X2 were identified as the KFs with the greatest impact on results, although in fact the X1/X2 ratio was the real cause. The results suggest that, with increased processing, the physical and chemical structure of lycopene becomes less important since the identified KFs explain almost 90% of variability in tomato paste but only 32% in raw tomato.  相似文献   

13.
Direct sample introduction (DSI) or "dirty sample injection" is a rapid, rugged, and inexpensive approach to large volume injection in gas chromatography (GC) for semivolatile analytes such as pesticides. DSI of complex samples such as eggs requires a very selective detection technique, such as tandem mass spectrometry (MS-MS), to determine the analytes among the many semivolatile matrix components that also appear. In DSI, the nonvolatile matrix components that normally would contaminate the GC system in traditional injection methods remain in a disposable microvial, which is removed after every injection. For example, 3 microg of nonvolatile residue typically remained in the microvial after an injection of egg extract using the DSI method. This analytical procedure involves the following: (i) weighing 10 g of egg in a centrifuge tube and adding 2 g of NaCl and 19.3 mL of acetonitrile (MeCN); (ii) blending for 1 min using a probe blender; (iii) centrifuging for 10 min; and (iv) analyzing 10 microL (5 mg of egg equivalent) of the extract using DSI/GC/MS-MS. No sample cleanup or solvent evaporation steps were required to achieve quantitative and confirmatory results with <10 ng/g detection limits for 25 of 43 tested pesticides from several chemical classes. The remaining pesticides gave higher detection limits due to poor fragmentation characteristics in electron impact ionization and/or degradation. Analysis of eggs incurred with chlorpyrifos-methyl showed a similar trend in the results as a more traditional approach.  相似文献   

14.
High-pressure processing (HPP) was utilized to induce unfolding of beta-lactoglobulin (beta-LG). beta-Lactoglobulin solutions at concentrations of 0.5 mg/mL, in pH 7.5 phosphate buffer, were pressure treated at 510 MPa for 10 min at either 8 or 24 degrees C. The secondary structure, as determined by circular dichroism (CD), of beta-LG processed at 8 degrees C appeared to be unchanged, whereas beta-LG processed at 24 degrees C lost alpha-helix structure. Tertiary structures for beta-LG, as determined by near-UV CD, intrinsic protein fluorescence spectroscopy, hydrophobic fluorescent probe binding, and thiol group reactivity, were changed following processing at either temperature. The largest changes to tertiary structure were observed for the samples processed at 24 degrees C. Model solutions containing the pressure-treated beta-LG showed significant decreases in surface tension at liquid-air interfaces with values of 54.00 and 51.69 mN/m for the samples treated at 24 and 8 degrees C, respectively. In comparison, the surface tension for model solutions containing the untreated control was 60.60 mN/m. Changes in protein structure during frozen and freeze-dried storage were also monitored, and some renaturation was observed for both storage conditions. Significantly, the sample pressure-treated at 8 degrees C continued to display the lowest surface tension.  相似文献   

15.
Toward the development of reliable qualitative and quantitative Polymerase Chain Reaction (PCR) detection methods of transgenic tomatoes, one tomato (Lycopersicon esculentum) species specific gene, LAT52, was selected and validated as suitable for using as an endogenous reference gene in transgenic tomato PCR detection. Both qualitative and quantitative PCR methods were assayed with 16 different tomato varieties, and identical amplified products or fluorescent signals were obtained with all of them. No amplified products and fluorescent signals were observed when DNA samples from 20 different plants such as soybean, maize, rapeseed, rice, and Arabidopsis thaliana were used as templates. These results demonstrated that the amplified LAT52 DNA sequence was specific for tomato. Furthermore, results of Southern blot showed that the LAT52 gene was a single-copy gene in the different tested tomato cultivars. In qualitative and quantitative PCR analysis, the detection sensitivities were 0.05 and 0.005 ng of tomato genomic DNA, respectively. In addition, two real-time assays employing this gene as an endogenous reference gene were established, one for the quantification of processed food samples derived from nontransgenic tomatoes that contained degraded target DNA and the other for the quantification of the junction region of CaMV35s promoter and the anti-sense ethylene-forming enzyme (EFE) gene in transgenic tomato Huafan No. 1 samples. All of these results indicated that the LAT52 gene could be successfully used as a tomato endogenous reference gene in practical qualitative and quantitative detection of transgenic tomatoes, even for some processed foods derived from transgenic and nontransgenic tomatoes.  相似文献   

16.
A liquid chromatographic (LC) method for determining tenuazonic acid (TA) and alternariol methyl ether (AME) in tomatoes and tomato products is described. The Alternaria metabolites are extracted from a water slurry of the sample with CHCl3, the mixture is centrifuged, and the extract is fractionated on a silica gel column. Reverse phase LC with an ultraviolet detector (for TA) and a fluorescence detector (for AME) connected in series is used for final separation and determination. The limit of determination for TA and AME is 25 and 3 ng/g, respectively, with average recoveries from catsup of 83 and 68%, respectively. The LC method also detects alternariol, but interfering peaks in some samples prevent accurate quantitation. Chemical ionization mass spectrometry (CIMS) is used to confirm TA. Samples (142) of tomatoes collected from commercial processing lines were analyzed; TA was found in 73 samples (0.4-70 micrograms/g).  相似文献   

17.
为研究不同均细化处理方式对桃果浆色泽的影响,本试验对新鲜桃原料进行打浆和超细粉碎(50 Hz)处理,对热烫后的桃原料进行打浆、胶体磨和湿法超细粉碎(18、26、34、42和50 Hz)处理,分析不同均细化处理对桃果浆表观色泽以及物质成分的影响.通过Pearson相关系数和逐步线性回归方程分析,进一步明确均细化处理过程中...  相似文献   

18.
Ten laboratories analyzed unfortified and fortified samples of lettuce, tomatoes, and strawberries for organochlorine and organophosphorus pesticides by applicable portions of the comprehensive multipesticide method of Luke et al. The 3 crops were fortified with 6 pesticides, alpha-BHC, dieldrin, chlorpyrifos, acephate, omethoate, and monocrotophos, each at 3 levels per crop. Included in the 54 fortifications were 16 pairs of blind duplicates: same pesticide, crop, and level. Recoveries were calculated by area comparisons with known reference materials, using the responses obtained from 2 separate element-specific gas chromatographic (GC) systems. The organochlorine pesticides were chromatographed on a methyl silicone column and detected with a Hall 700A electrolytic conductivity detector, and the organophosphorus pesticides were determined with a flame photometric detector after being chromatographed on a specified DEGS column material. Chlorpyrifos was quantitated on both GC systems. Mean recoveries ranged from 82.6% for acephate fortified at 0.5000 ppm in strawberries to 118.1% for 0.0636 ppm fortification of chlorpyrifos in lettuce. Interlaboratory coefficients of variation ranged from 4.0% for 0.6360 ppm fortification of chlorpyrifos in tomatoes to 17.8% for the 0.0636 ppm chlorpyrifos level in lettuce. The procedure features essentially no cleanup before GC and proved comparable to existing multiresidue methods for pesticides of the class types studied, as evidenced by the intra- and interlaboratory measurements of precision and recoveries obtained. The method with the 2 GC systems has been adopted official first action.  相似文献   

19.
The processing factors (pesticide concentration found in olive oil/pesticide concentration found in olives) of azinphos methyl, chlorpyrifos, lambda-cyhalothrin, deltamethrin, diazinon, dimethoate, endosulfan, and fenthion were determined in olive oil production process in various laboratory-scale olive oil extractions based on three- or two-phase centrifugation systems in comparison with samples collected during olive oil extractions in conventional olive mills located at different olive oil production areas in Greece. Pesticide analyses were performed using a multiresidue method developed in our laboratory for the determination of different insecticides and herbicides in olive oil by solid-phase extraction techniques coupled to gas chromatography detection (electron capture detection and nitrogen phosphorus detection), optimized, and validated for olive fruits sample preparation. Processing factors were found to vary among the different pesticides studied. Water addition in the oil extraction procedure (as in a three-phase centrifugation system) was found to decrease the processing factors of dimethoate, alpha-endosulfan, diazinon, and chlorpyrifos, whereas those of fenthion, azinphos methyl, beta-endosulfan, lambda-cyhalothrin, and deltamethrin residues were not affected. The water content of olives processed was found to proportionally affect pesticide processing factors. Fenthion sulfoxide and endosulfan sulfate were the major metabolites of fenthion and endosulfan, respectively, that were detected in laboratory-produced olive oils, but only the concentration of fenthion sulfoxide was found to increase with the increase of water addition in the olive oil extraction process.  相似文献   

20.
Commercial food processing operations such as washing, blanching, and cooking remove major portions of the pesticide residues that are currently permitted on the raw agricultural crop. These unit operations are reviewed for selected products, along with degree of residue removal at each step. For example, washing plus peeling removes 99% of carbaryl and malathion residues from tomatoes. Washing removes 83% of benomyl residue from tomatoes and further processing reduces the residue by 98% in tomato puree and catsup. Even in the most concentrated fraction from tomatoes (tomato paste), residues were below the initial level in the raw product.  相似文献   

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