共查询到20条相似文献，搜索用时 310 毫秒
1.
D W Fink A Fox J V Pivnichny 《Journal of the Association of Official Analytical Chemists》1979,62(1):1-4
Arprinocid [9 - (2 - chloro - 6 - fluorophenylmethyl)-9H-purin-6-amine] is determined in feed by high pressure liquid chromatography with a silica column and ultraviolet detection. The drug is extracted from the feed into chloroform in the presence of pH 7 phosphate buffer, transferred to 0.1N HCl, and separated from interfering substances by partitioning with hexane. The acidic solution is neutralized, and the analyte is extracted into chloroform for injection into the chromatograph. This procedure has been applied to feeds containing 0.0030--0.0090% arprinocid with a precision of less than 5% relative standard deviation at the 0.0060% formulated concentration level. The results of this chromatographic procedure also correlate with those from a colorimetric analysis. 相似文献
2.
L S Cottingham R L Smallidge 《Journal of the Association of Official Analytical Chemists》1988,71(5):1012-1016
A sample portion is hydrolyzed with 6N HCl for 23 h and cooled, the pH is adjusted to 7.7 with NaOH, and the solution is diluted with pH 7.7 borate buffer. An aliquot of the sample extract is derivatized with 9-fluorenylmethyl chloroformate (9-FMC). Lysine is separated from other amino acids by isocratic reverse-phase liquid chromatography (LC) using fluorescence detection: 260 nm excitation and 313 nm emission. The mobile phase is acetonitrile-0.1M acetic acid (pH 4.2) buffer (53 + 47). Linearity is satisfactory over a range of 0.4-24 micrograms/mL. Results from 9 feed samples (1.1-2.7% lysine) analyzed by both the LC method and an amino acid analyzer were not significantly different statistically. Recovery of standard lysine, spiked just before derivatization on these same 9 samples (in duplicate), was 100.9% with a coefficient of variation (CV) of 2.4%. A study of within-day and between-day method precision resulted in CVs of 1.1 and 1.8%, respectively. The variation of results was negligible when the method was tested for ruggedness on 7 factors. 相似文献
3.
G Shah D Bradley E Shek 《Journal of the Association of Official Analytical Chemists》1984,67(4):707-714
A relatively simple analytical method is presented for determination of oxfendazole (2-(methoxycarbonylamino)-5-phenylsulfinyl-benzimidazole) at levels as low as 0.012% in swine feeds, using cation exchange liquid chromatography (LC). The sample was extracted with a solvent mixture of methanol-glacial acetic acid (90 + 10) at 45 degrees C, using a gyrorotory shaker. Plant pigments and other feed excipients were removed using zinc acetate treatment and pH-controlled extraction. Oxfendazole was further separated from the remaining interferences and quantitatively determined by LC on a Partisil SCX column with acetonitrile-0.01M phosphate buffer as mobile phase. The method is stability-specific, linear, precise, and accurate at 80-120% labeled strength (relative standard deviation 0.9-1.7 with mean recovery of 98-99%). Supporting data at a level of 0.0135% oxfendazole in swine feed indicated that this method is capable of complete recovery of oxfendazole from medicated swine feeds. 相似文献
4.
In this work, soy protein isolates were produced by a combination of electroacidification and high shear tangential flow hollow fiber ultrafiltration with a 100 kDa membrane under constant pressure. The filtration performance was evaluated by comparing the filtration time and the final product composition for an electroacidified (pH 6) and a non-electroacidified (pH 9) soy protein extract. The removal of carbohydrates during the filtration was always consistent with the theoretical predictions (based on free permeability assumption) for both the electroacidified and the non-electroacidified feeds. A higher removal of calcium, magnesium, and phytic acid was achieved during the filtration of the electroacidified feed compared to the non-electroacidified feed. However, the electroacidification pretreatment had a negative impact on the permeate flux and resulted in more significant membrane fouling with correspondingly longer filtration times. A discontinuous diafiltration enhanced the removal of carbohydrates and minerals, thus yielding a product with higher protein content but was unable to improve the permeate flux for the electroacidified feed. 相似文献
5.
S J Doherty A Fox D W Fink 《Journal of the Association of Official Analytical Chemists》1990,73(6):931-934
An analytical method has been developed that is applicable to the determination of Ivermectin in medicated feeds at the 2 ppm concentration level. It is based upon liquid chromatographic analysis with a reverse-phase column and ultraviolet detection. After the drug is extracted from the feed into methanol, an analytical sample is prepared by the consecutive use of column chromatography on alumina and solid-phase extraction on Sep-Pak C18 and silica cartridges. This procedure has been applied to the concentration range 0.50-3.0 ppm of Ivermectin in feed with an accuracy of +/- 2% mean relative error and a precision of +/- 2% relative standard deviation at the 2 ppm concentration level. 相似文献
6.
基于高光谱成像技术的青贮玉米饲料pH值无损检测 总被引：1，自引：1，他引：0
为实现青贮玉米饲料pH值的快速、无损检测,该研究采用高光谱成像技术建立不同品质青贮玉米饲料pH值的定量检测模型。采集青贮玉米饲料样本936～2 539nm的平均光谱,采用6种预处理方法对青贮玉米饲料平均光谱进行处理,通过建立偏最小二乘回归（partialleastsquaresregression,PLSR）模型得出多元散射校正（multiplicativescatter correction,MSC）和卷积平滑（savitzky-golay,SG）两种预处理方法效果较好,使用竞争性自适应重加权算法（competitive adaptive reweighted sampling,CARS）、变量组合集群分析算法（variable combination population analysis,VCPA）以及迭代保留信息变量（iteratively retains informative variables,IRIV）算法对经MSC和SG卷积平滑预处理光谱进行特征波长提取,利用PLSR和极限学习机（extreme learning machines,ELM）分别建立饲料全波段、特征波长... 相似文献
7.
M C Allred J L MacDonald 《Journal of the Association of Official Analytical Chemists》1988,71(3):603-606
Samples of 4 foods, 1 animal feed, isolated soy protein, and beta-lactoglobulin were analyzed by 9 laboratories to determine concentrations of cysteine as cysteic acid, methionine as methionine sulfone, and tryptophan. Sulfur amino acids were determined by AOAC method 43.A08-43.A13 for food and feed ingredients, in which samples are oxidized with performic acid before protein hydrolysis with 6N HCl. Tryptophan was determined after protein hydrolysis with 4.2N NaOH. In both methods, free amino acids were separated by ion-exchange or reverse-phase chromatography. Each laboratory was provided with detailed methods and with sealed vials containing solutions of standards. Samples were analyzed in duplicate, and variation between laboratories was determined. Coefficients of variation between laboratories for the 6 samples ranged from 5.50 to 11.8% for methionine as methionine sulfoxide, 8.59 to 17.3% for cysteine as cysteic acid, and 3.87 to 16.1% for tryptophan. Amino acid recoveries were determined by analysis of beta-lactoglobulin and were based on expected levels of each amino acid obtained from amino acid sequence data. The mean recovery of cysteine was 97% with a range of 88-119%. For methionine, mean recovery was 98% (range 89-115%) and for tryptophan, 85% (range 59-102%). Method 43.A08-43.A13 for food and feed ingredients has been adopted official first action for determination of cysteine and methionine in processed foods. The alkaline hydrolysis method has been adopted official first action for determination of tryptophan in foods and food and feed ingredients. 相似文献
8.
Mechanisms controlling zinc solubility in soils 总被引：1，自引：0，他引：1
I.D. PULFORD 《European Journal of Soil Science》1986,37(3):427-438
The removal of zinc from solution has been studied for seven soils of varying properties. The presence of a background electrolyte as an ionic strength buffer and the nature of the anions and cations in solution have also been examined. This process has been considered as both a surface adsorption and a precipitation mechanism. Evidence presented suggests a role for a precipitation mechanism involving zinc and iron, which is independent of pH. Iron concentration in solution decreased with increasing zinc concentration; the ion product pZn+2pFe was constant (15.00, SD 1.00) over all seven soils. A further indicator of a precipitation mechanism was the shape of the Langmuir plot at low equilibrium concentrations of zinc in solution. 相似文献
9.
Schwenke KD Mothes R Dudek S Görnitz E 《Journal of agricultural and food chemistry》2000,48(3):708-715
The effect of progressive phosphorylation by phosphorous oxychloride upon the conformation of the 300 kDa storage protein (cruciferin) from rapeseed has been studied using chemical analysis, SDS-PAGE, HPLC, analytical ultracentrifugation, viscometry, fluorescence spectroscopy, and hydrophobicity measurement. The amount of phosphorous in the protein increased with the excess of phosphorous oxychloride and the pH of reaction. The bulk of phosphorus was only loosely bound to the protein and was removed by washing with cold perchloric acid. The more stably bound phosphorus groups after reaction at pH 8 were found to be nearly equally attached to amino and hydroxyl groups, whereas phosphorylation at pH 10-11 led to predominant O-phosphorylation as detected by studying the acid- and alkali-lability of the protein-phosphorous bonds. A 50 kDa component appeared as a product of covalent cross-linking of the constituent alpha- and beta-polypeptide chains. A 2.5S fraction appeared as the main product of dissociation, which takes place after a critical step of modification. The higher the extent of phosphorylation, the larger was the percentage of higher molecular weight products, the percentage of which was most significant after modification under strongly alkaline conditions. They may be attributed both to products of chemical cross-linking and to noncovalently linked aggregates formed by interactions of partially unfolded derivatives exhibiting an increased surface hydrophobicity. 相似文献
10.
Mondor M Ippersiel D Lamarche F Boye JI 《Journal of agricultural and food chemistry》2004,52(23):6991-6996
Soy protein concentrates produced by combining electroacidification and dead-end ultrafiltration with a membrane of 100 kDa (pH 7 and 6) were compared with concentrates produced by ultrafiltration (pH 9) and a traditional acid precipitation procedure at pH 4.5. Mineral removal during ultrafiltration (mainly potassium, phosphorus, and calcium) was enhanced for the pH 6 electroacidified extract, compared to the extract at pH 9. This yielded a concentrate with improved solubility characteristics. The solubility for the concentrate prepared at pH 6 was enhanced by as high as 45% when compared to the concentrate at pH 9. The concentrate produced according to the traditional acid precipitation process showed mineral contents and solubility profile similar to those of the pH 6 concentrate, but required twice as much water during the process. The effect of electroacidification treatments on ultrafiltration permeate flux was quantified through the measurement of the different hydraulic resistances. Cake resistance was the main resistance to the permeate flux, and it was minimum at pH 9, maximum at pH 7, and intermediate at pH 6. 相似文献
11.
12.
Starkenmann C 《Journal of agricultural and food chemistry》2003,51(24):7146-7155
Cysteine conjugates, resulting from the addition of cysteine to alpha,beta-unsaturated carbonyl compounds, are important precursors of odorant sulfur compounds in food flavors. The aim of this work was to better understand this chemistry in the light of the unexpected double addition of cysteine to two unsaturated aldehydes. These reactions were studied as a function of pH. When (E)-2-methyl-2-butenal (tiglic aldehyde, 4) was treated with cysteine in water at pH 8, the major product formed was the new compound (4R)-2-(2-[[(2R)-2-amino-2-carboxyethyl]thio]methylpropyl)-1,3-thiazolidine-4-carboxylic acid (6). Under acidic conditions (pH 1), we also observed a double addition, but the second cysteine was linked by a vinylic sulfide bond to form the previously unreported major product, (2R,2'R,E)-S,S'-(2,3-dimethyl-1-propene-1,3-diyl)bis-cysteine (7). When (E)-2-hexenal (12) was treated with cysteine under acidic conditions, the major product was the novel (4R,2' 'R)-2-[2'-(2' '-amino-2' '-carboxyethylthio)pentyl]-1,3-thiazolidine-4-carboxylic acid (13), and the formation of an vinylic sulfide compound analogous to 7 was not observed. Reduction of the acidic crude reaction mixture with NaBH(4) afforded 13 and the cysteine derivative (R)-S-[1-(2-hydroxyethyl)butyl]cysteine (14) in 14% yield. Treating (E)-2-hexenal with cysteine at pH 8 followed by NaBH(4) reduction yielded the new product (3R)-7-propylhexahydro-1,4-thiazepine-3-carboxylic acid (15). Addition of cysteine to mesityl oxide (16), at pH 8, followed by reduction with NaBH(4) furnished (R)-S-(3-hydroxy-1,1-dimethylbutyl)cysteine (3) and the new compound (3R)-hexahydro-5,7,7-trimethyl-1,4-thiazepine-3-carboxylic acid (18). 相似文献
13.
L J Nu?ez-Vergara J A Squella E M Gonzalez 《Journal of the Association of Official Analytical Chemists》1979,62(3):556-559
A polarographic method has been developed for the quantitative analysis of cephradine and its dosage forms. Direct determinations on capsules are carried out; excipients and coloring matter do not interfere in the determination. The electroactive product is formed by acidic hydrolysis with 5.0N HCl and heating at 80 degrees C for 60 min. Two polarographic waves are obtained: I = -0.46 V and II = -0.78 v vs. SCE. Both reduction waves are diffusion controlled. Wave I is preferred for analytical purposes. The precise chemical identity of the electroactive product has not been determined, but UV spectral data and the TLC Rf value are reported. A linear relation is established for levels of cephradine between 10(-2) and 10(-5)M in 5.0N HCl. 相似文献
14.
Daniel MA Elsey GM Capone DL Perkins MV Sefton MA 《Journal of agricultural and food chemistry》2004,52(26):8127-8131
Damascenone has been shown to undergo reaction with common wine components. Following the action of acid and heat alone, two bicyclic compounds, 4,9,9-trimethyl-8-methylenebicyclo[3.3.1]non-6-en-2-one (2) and 4,4,9-trimethyl-8-methylenebicyclo[3.3.1] non-6-en-2-one (3), were isolated. However, this conversion takes place only very slowly, if at all, under milder conditions (45 degrees C). When treated with a variety of nucleophiles at pH 3.0 and 5.5, the concentration of damascenone in buffered aqueous ethanol decreased by minor amounts (10-20%) except for cysteine and 2-mercaptoethanol addition at pH 5.5 (approximately 40 and approximately 30%, respectively) and SO2 (>90% at pH 3.0; 100% at pH 5.5). An adduct from this last combination was prepared and shown to be the C9 sulfonic acid derivative of damascenone. A detailed investigation into the effect of SO2 demonstrated that loss of damascenone in model wine was directly related to the concentration of added SO2 but was essentially unaffected by small changes in pH. 相似文献
15.
B Ramaroson-Raonizafinimanana E M Gaydou I Bombarda 《Journal of agricultural and food chemistry》1999,47(8):3202-3205
Analyses of the neutral lipids from Vanilla species before saponification resulted in the identification of a new product family in this genus: long-chain gamma-pyrone compounds with an aliphatic chain containing a cis double bond at the n-9 position. These compounds represent 7-8% of the neutral lipids in mature beans. Using NMR and gas chromatography/mass spectrometry, three gamma-pyrones have been identified, including 2-(10-nonadecenyl)-2, 3-dihydro-6-methyl-4H-pyran-4-one, 2-(12-heneicosenyl)-2, 3-dihydro-6-methyl-4H-pyran-4-one, and 2-(14-tricosenyl)-2, 3-dihydro-6-methyl-4H-pyran-4-one. The major constituent was 2-(14-tricosenyl)-2,3-dihydro-6-methyl-4H-pyran-4-one, which represented 70.3% of the gamma-pyrone fraction. The variability of this compound family has been studied in relation to bean maturity in V. fragrans and V. tahitensis beans. This compound family has not been found either in leaves or in stems or in V. madagascariensis beans. 相似文献
16.
污染场地开挖置换后的污染土经过固化处理（S/S法）,可作为浅层地基或护岸等非敏感区域的建筑材料,进行污染土的二次利用。针对该项技术,将一定量硝酸锌溶液与风干后红粘土混合,掺入适量水泥,并搅拌均匀、压实成型,标准养护7 d和28 d后依次进行无侧限抗压实验、压汞实验和含水率、体积等指标的测定,研究不同锌离子浓度、水泥掺量和养护龄期对锌污染红粘土水泥固化产物强度、微观孔隙和含水率等的影响。实验结果表明：水泥掺量在10%以内,锌离子浓度小于5000 mg·kg-1,固化物强度随龄期增长而增加;锌离子浓度大于5000 mg·kg-1,强度随龄期增长而先增加后减小。水泥掺量6%和8%时,固化物强度与锌离子浓度呈负相关;而水泥掺量10%时,锌离子浓度对强度的影响存在阈值,且阈值在1000 mg·kg-1附近。与不含锌离子的28 d固化物相比,锌离子浓度小于1000 mg·kg-1时,固化产物孔径小于10 nm的孔隙增加,孔径大于10μm的孔隙减少,强度提高;锌离子浓度在大于1000 mg·kg-1时,严重阻碍C-S-H凝胶物的生成,10μm以上的孔隙和总孔隙率均显著增加,并且生成大量孔径为0.1~10μm的无定型物,同时使红粘土出现亲水性,养护过程中吸收水分且体积增加,强度则大幅度降低。 相似文献
17.
Puglisi CJ Daniel MA Capone DL Elsey GM Prager RH Sefton MA 《Journal of agricultural and food chemistry》2005,53(12):4895-4900
A series of four isomeric 3,9-dihydroxymegastigma-4,6,7-trienes, 8, has been prepared. The (3S,6R,9S) isomer of 8 proved to be identical to an isomer of this compound tentatively identified as an intermediate in the formation of damascenone from an allene triol. Each of the four isomers, when hydrolyzed independently of each other at pH 3.0 and 25 degrees C, produced product mixtures in which the major product was damascenone (1). Contrary to expectation, 3-hydroxydamascone (5) was not observed in any of the hydrolyses. Consequently, the mechanism of formation of damascenone proposed earlier requires modification. In each hydrolysis, the product mixtures showed the presence of a second isomer of 8, produced by epimerization during hydrolysis. Chiral analysis on a Cyclosil B column revealed that this epimerization was occurring at C(3) in each of the hydrolyses. 相似文献
18.
Malik AK Sharma V Sharma VK Rao AL 《Journal of agricultural and food chemistry》2004,52(26):7763-7767
A procedure has been developed for the determination of zinc(II) bis(dimethyldithiocarbamate) (ziram) and zinc(II) ethylenebis(dithiocarbamate) (zineb) after preconcentration on a column using naphthalene-(1,2'-pyridylazo)-2-naphthol (PAN) as adsorbent. Ziram and zineb are quantitatively retained on the column in the pH range of 9.0-12.5 and at a flow rate of 1-2 mL/min. The solid mass consisting of the Zn-PAN complex along with naphthalene is dissolved from the column with 5 mL of dimethylformamide (DMF). Absorbance of the complex was measured at 550 nm; Beer's law is obeyed over the concentration ranges of 2.0-22.0 microg of ziram and 5.0-19.8 microg of zineb in 10 mL of the final DMF solution. Ten replicate determinations on a sample solution containing 20 microg of ziram and 18 microg of zineb gave a mean absorbance of 0.33 with relative standard deviations of 0.80 and 0.70%, respectively. The interference of various ions has been studied. The method has been employed for the determination of ziram and zineb in commercial samples and in various foodstuffs, and the results were compared with the earlier reported methods. 相似文献
19.
For the preparation of amino acid chelated fertilizer, chicken feathers were hydrolyzed with sulfuric acid (H2SO4; 6M) and potassium hydroxide (KOH; 6M) separately in the presence of different catalysts. Under acidic conditions, the catalyst zinc sulfate, gave minimum ammonium but a maximum conversion rate of organic nitrogen (N) into amino acids (19% higher than control). Under alkaline conditions, sodium sulfide showed maximum amino acid-N and conversion rate (37% higher than control). The catalyst doses showed a continuous increase in the conversion rate and were highest at 12%. The ratio of 1:3 feathers: hydrolytic agent showed maximum conversion rate. Hydrolytic time had a nonsignificant effect under acidic conditions, but under alkaline conditions a hydrolytic time of 14 h gave the maximum conversion rate. The chelation experiment results showed that the ratios (2:1, 2.5:1, and 3:1) showed almost equal chelation rates, except the 1:1 ratio of hydrolysis product to salt. Iron (Fe), copper (Cu), and manganese (Mn) showed maximum chelation rates under acidic pH, while zinc (Zn) showed maximum chelation rate at an alkaline pH. Temperature and chelation time had a nonsignificant effect on chelation rate. Comparative study results of amino acid chelated Zn and Fe fertilizers, ethylenediaminetetraacetic acid (EDTA) chelated Zn and Fe fertilizers, and zinc sulfate (ZnSO4) and iron sulfate (FeSO4) fertilizer foliar application to upland rice showed that a 1/100 dilution of amino acid chelated Zn and Fe fertilizers increased growth parameters from 22–73%, while EDTA chelated Zn and Fe fertilizers caused an increase of 15–63%, and ZnSO4 and FeSO4 increased growth parameters from 11–35% over the control. After fertilizer application, increase in chlorophyll contents was 11–17%, 3–6%, and 8–12%, respectively, over control. Therefore, amino acid chelated micronutrient fertilizer is used in small amounts, has a low cost, and high rates of return. 相似文献
20.
Yamazaki S Iwasa K Kano K Ikeda T Taketomo N Kaneko T 《Journal of agricultural and food chemistry》2000,48(11):5643-5648
Nonenzymatic reduction of dehydroascorbate into ascorbate by the reduced form (quinol form) of 2-amino-3-carboxy-1,4-naphthoquinone, a strong growth stimulator for bifidobacteria, has been found. The bimolecular reaction rate constant was evaluated as 9 M(-)(1) s(-)(1) at pH 7.0. This reaction has been successfully coupled with enzymatic regeneration of the naphthoquinol by NAD(P)H in cell-free extracts of Bifidobacterium longum 6001. The overall reaction is a regeneration of NAD(P)(+) by dehydroascorbate [or a regeneration of ascorbate by NAD(P)H], in which the naphthoquinone/quinol redox couple functions as an electron transfer mediator. Kinetic study of the reduction of dehydroascorbate with related quinol compounds suggested the significance of the amino substituent of the naphthoquinol. A mechanism of the electron transfer from the quinol to dehydroascorbate is proposed, where the first step of the reaction is a nucleophilic addition of the C(2)-amino substituent of the naphthoquinol to the C(2)-position of dehydroascorbate to form a Schiff base intermediate. 相似文献