Nitrate determination in baby food, using the nitrate ion selective electrode.

The nitrate electrode has been utilized in the determination of nitrate content in food products. The AOAC xylenol method was employed for comparative results. A reasonable correlation (r=0.91) was found between the 2 methods in the analysis of 49 samples containing 30-350 ppm nitrate. At the average nitrate content (100 ppm) of these foods, the standard error was 4.3 ppm. The electrode responds directly to the ionic activity of the nitrate ion. It has a linear concentration range of 1-6000 ppm nitrate and can be used over a wide pH range. The electrode does respond to some extent to anions other than nitrate, and some interferences do occur. These interferences are easily controlled by the use of cation exchange resins. The Corning known addition (spiking) method is used on all samples to insure correct electrode response in solutions containing variable background ionic composition. The electrode has the advantage of simplicity, speed, reproducibility, and accuracy. Work time saved using the electrode as opposed to the xylenol method is about 7 hr for the analysis of 20 samples. Error, and the need for repeating analysis, is much less frequent.     

Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography

Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.     

刮盐皮-标准曲线法测土壤盐分与其他方法的比较

测定土壤中可溶性盐分有不同的方法,残渣烘干法为经典法,适用于不同土壤;阴阳离子总和测定法误差稍大,操作较繁;电导法-标准曲线法如果标准样品少,精确度达不到要求;刮盐皮—标准曲线法有较好的实用性,在一定地域内可以进行土壤可溶性盐分的快速测定,精确度准确可靠。     

Development of an immunoassay (ELISA) for the quantification of thiram in lettuce

Two competitive immunoassays, a laboratory assay based on microwell plates and a field test based on the use of polystyrene tubes, have been developed for the quantification of thiram in lettuces. Concerning the laboratory assay, the calibration curve for thiram had a linear range of 11 to 90 ng/mL and a detection limit of 5 ng/mL. Precision of the assay presented coefficient of variation values <9% and the recovery of thiram from lettuce averaged 89% across the range of the immunoassay method using 30 min extraction with water/acetone (50:50, v/v). The tube-based method was developed in order that an extract of lettuce, containing thiram at the MRL (8 ppm), would be found on the linear part of the standard curve. The calibration curve for thiram has a linear range of 100 to 800 ng/mL (1.39 to 11.1 ppm in lettuce) and a detection limit of 40 ng/mL.     

Determination of linuron in potatoes using capillary column gas chromatography/mass spectrometry

A convenient method for the determination of the N-methyl,N-methoxy-phenylurea herbicide (linuron) in potatoes has been developed. The herbicide is extracted from potatoes using a slightly modified Luke multiresidue procedure. The extract is analyzed directly by gas chromatography with cold on-column injection, using an ion trap mass spectrometer in the chemical ionization mode as the detector. Quantitation is performed using p-bromonitrobenzene as the internal standard. The limit of detection is 0.1 ppm. Recoveries of linuron in potatoes averaged 112 +/- 6% at the 0.5 ppm level, and 110 +/- 2% at the 0.2 ppm level. No linuron residues were found in 25 potato samples that were analyzed by this method. Two other N-methyl,N-methoxy-phenylurea herbicides, metobromuron and chlorbromuron, are also sufficiently stable to be determined by this method, but the N,N-dialkyl-phenylurea herbicides neburon, diuron, and monuron are too thermally unstable and degrade in the gas chromatograph.     

Effect of pH Conditions on Actual and Apparent Fluoride Adsorption by Biochar in Aqueous Phase

Biochar is a carbon-rich product derived from biomass through pyrolysis. Fluoride adsorption potential of the biochar derived from orange peel (OP) and water treatment sludge (WS) at different pyrolytic temperatures (400, 600, and 700?°C) was investigated in a batch mode as a function of pH. With respect to adsorption, two types were considered, i.e., actual and apparent adsorption where fluoride combined with metal complexes in solution were counted and not counted, respectively. The highest actual fluoride adsorption was observed in the pH range of 2.0 to 3.9 for OP biochar and 5.1 to 6.2 for WS biochar, respectively. For the WS biochar, apparent fluoride adsorption showed nearly 100?% in the pH range of 2.0 to 4.5, and then the adsorption capacity diminished drastically as the pH increased from 5.0 to 10.0. There was no significant difference between apparent and actual fluoride adsorption for OP biochar. In the Fourier-transform infrared spectroscopic analysis of WS biochar, a strong and sharp band was observed at around 2,364?cm^?1 after adsorption of fluoride. Elemental content analysis by the energy-dispersive X-ray method revealed that the fluorine content was higher at pH 6.0 than at pH 3.0 and 9.0 as the results of actual fluoride adsorption. From these results, we may conclude that the biochar derived from OP and WS can be reused as an economical and effective adsorbent for fluoride removal in acidic aqueous phase.     

Monitoring of feeds selenium status in a southeast region of Romania

One hundred and eighty-five samples of feeds (hays, green plants, and concentrate feed) from households covering 41 localities in Dobrudja, a southeast region of Romania, were collected and analyzed for selenium (Se) content by spectrofluorometry with 2,3-diaminonaphthalene. Only 6.5% of the samples analyzed were, in terms of the feed Se content, considered appropriate (i.e., 0.15-0.30 ppm), within the normal range. The remaining 93.5% proved to be Se deficient; the results fell into the 0.001-0.150 ppm range. Consequently, the samples were divided into three deficiency groups based on the content recorded as follows: severe for 3.2% (Se below 0.01 ppm), critical for 84.9% (Se in the 0.01-0.1 ppm range), and marginal for 5.4% (Se in the 0.1-0.15 ppm range). Conclusively, the Dobrudja feeds may be said to be generally Se deficient, which requires prophylactic and therapeutic measures to correct animal selenium deficiency.     

Visual immunoassay for detection of Salmonella in foods: collaborative study

A collaborative study was performed in 13 laboratories to validate a visual enzyme immunoassay (EIA) procedure, TECRA, for rapid detection of Salmonella in foods. The EIA method was compared with the standard culture procedure for detection of Salmonella in 6 food types: ground black pepper, soy flour, dried whole eggs, milk chocolate, nonfat dry milk, and raw deboned turkey. Uninoculated and inoculated samples were included in each food group analyzed. There was no significant difference in the productivity of the EIA and culture procedures at the 5% level for any of the 6 foods. The enzyme immunoassay screening method has been approved interim official first action.     

DNA hybridization assay for detection of Salmonella in foods: collaborative study

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.     

Gas chromatographic/mass spectrometric determination of daminozide in high protein food products

A gas chromatographic/mass spectrometric (GC/MS) method for determining daminozide in high protein products has been developed. Daminozide is hydrolyzed in the presence of a strong base to form unsymmetrical dimethylhydrazine (UDMH) which is then distilled from the food matrix. A stable derivative is formed by reacting UDMH with salicyladehyde to form salicyaldehyde dimethylhydrazone. This derivative is separated and quantitated by GC/MS using selected ion monitoring (SIM) of key ions in the fragmentation pattern: m/z 164 (molecular ion of hydrazone) and m/z 120 (C7H6ON). An internal standard, 4-nitroanisole, is monitored at m/z 153 (molecular ion) and m/z 123 (C6H5O2N). The limit of detection is 0.01 ppm daminozide in a 50 g sample; however, because of variation at low levels, the limit of quantitation is 0.1 ppm. Recoveries are 90% or greater from peanuts and peanut butter spiked at the 0.1-2 ppm level. Reproducibility of the method depends on the food matrix and is 26% RSD in the worst case. Data are compared for the GC/MS method and the official EPA colorimetric procedure. Results showed a high bias in the colorimetric method, especially when roasted peanut products were analyzed.     

Determination of ivermectin in medicated swine feeds at the 2 ppm concentration level

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.     

Fluorescent enzyme immunoassay for rapid screening of Salmonella in foods: collaborative study

A collaborative study was performed in 13 laboratories to validate an enzyme immunoassay (EIA) procedure for rapid detection of Salmonella in foods. The EIA was compared with the standard culture procedure for detection of Salmonella in 6 food types: ground black pepper, soy flour, dried whole eggs, milk chocolate, nonfat dry milk, and raw deboned turkey. Uninoculated and inoculated samples were included in each food group analyzed. There was no significant difference in the proportion of samples positive by the EIA and culture procedures at the 5% level for any of the 6 foods. The enzyme immunoassay screening method has been adopted official first action as a rapid screening method for detection of Salmonella.     

Die potentiometrische Bestimmung von Nitrat im Boden mit einer Membranelektrode

Soil-Nitrate Determination with the NO₃-sensitive Electrode A NO₃-sensitive ion electrode (Orion, No. 92–07) was tested to determine the nitrate concentration in soil extracts. Some analytical problems are to be respected: 2. During a 2–8 week period of measurement the electrode gradually lost its potential (Figure 2). Therefore it is necessary to replace the sensitive elements (ion-exchanger, nitrate concentration and membran of electrode) at a certain level (in this 165 mV with 0.22 ppm NO,-N-solution). 3. Additional problems are from the heterogenity of thes oil(s = 0.10mg NO₃-N/100g soil in this experiment). With 4 replications in sampling at given site or date, significant differences in the range of 20 kg NO,-N/ha have been obtained. Observing the before mentioned precautions the correlation between nitrate content 1. The optimal range for measurements can be calculated by application of the Peters-Nernst equation between 1 to 10 ppm NO₃-N (Figure 1). This equation is influenced by the used electrode. Because this influence changed, it is necessary, to measure the standard solution before and after the series. determined by the nitrate electrode and conventional method (r = 0.92, Figure 3) was highly significant. The deviation of 0.28 ppm has no influence on the agronomy conclusions based on the nitrate determinations.     

Use of lignin extracted from different plant sources as standards in the spectrophotometric acetyl bromide lignin method

A nongravimetric acetyl bromide lignin (ABL) method was evaluated to quantify lignin concentration in a variety of plant materials. The traditional approach to lignin quantification required extraction of lignin with acidic dioxane and its isolation from each plant sample to construct a standard curve via spectrophotometric analysis. Lignin concentration was then measured in pre-extracted plant cell walls. However, this presented a methodological complexity because extraction and isolation procedures are lengthy and tedious, particularly if there are many samples involved. This work was targeted to simplify lignin quantification. Our hypothesis was that any lignin, regardless of its botanical origin, could be used to construct a standard curve for the purpose of determining lignin concentration in a variety of plants. To test our hypothesis, lignins were isolated from a range of diverse plants and, along with three commercial lignins, standard curves were built and compared among them. Slopes and intercepts derived from these standard curves were close enough to allow utilization of a mean extinction coefficient in the regression equation to estimate lignin concentration in any plant, independent of its botanical origin. Lignin quantification by use of a common regression equation obviates the steps of lignin extraction, isolation, and standard curve construction, which substantially expedites the ABL method. Acetyl bromide lignin method is a fast, convenient analytical procedure that may routinely be used to quantify lignin.     

Comparison of Conductimetric and Colorimetric Methods with Distillation–Titration Method of Analyzing Ammonium Nitrogen in Total Kjeldahl Digests

The distillation–titration method (DTM) is a standard procedure used by most laboratories to measure ammonium-nitrogen (NH₄-N) in the total Kjeldahl N (TKN) digests of various kinds of agricultural and environmental samples. These samples may have TKN contents ranging from less than 100 ppb to as high as percentage levels. However, the DTM procedure generally leads to a very low throughput because it is labor intensive and time-consuming. At the current practical quantitation limit (PQL) of 300 ppb established at the Feed and Environmental (FEW) Laboratory, University of Georgia, the DTM procedure is less applicable to low TKN surface water samples. In this study, we therefore compared the performance of diffusion conductivity method (DCM) and colorimetric method (CM) with DTM in measuring NH₄-N in the TKN digests of 29 different samples representing surface waters, lagoons, manures, poultry litters, and environmental wastes. Acceptable accuracy and precision were achieved for various QC samples by all three methods. For widely different sample matrices and TKN contents, the NH₄-N in the TKN digests measured by DCM and CM both agreed well with that measured by DTM. However, the linear working range of CM is limited within 0.2 to 5.0 ppm, whereas DCM is linear at a wider range of 0.01 to 2000 ppm. With DCM, the PQL of TKN is at 13 ppb, much less than the 300 ppb in DTM and 520 ppb in CM. Both DCM and CM require increasing the pH of the working TKN digest to a highly alkaline range. To meet such pH requirement, the minimum dilution need for DCM is twofold, where as that CM is fourfold. Because of greater mandatory dilution requirement coupled with a greater PQL, CM may often fail to measure NH₄-N in the working TKN digest of some low TKN surface water samples. On the other hand, with some environmental waste samples containing TKN at percentage level, CM would require multistep dilution of the digests prior to measurement, thus allowing dilution-related error as well as requiring additional labor. In contrast, DCM can measure both low TKN surface waters and high TKN environmental wastes without any major limitations. Moreover, DCM may work well without any adjustment of sample background in the calibration standards. Thus DCM appears to be an attractive alternative to the labor-intensive and time-consuming DTM for measuring NH₄-N in the TKN digests of various kinds of agricultural and environmental samples in the analytical services laboratories.     

SOIL FLUORINE

The development of techniques for measuring soluble and labile soil fluoride using a specific-ion fluoride electrode are described. The methods evolved were used to assess the fluoride status of numerous agricultural soil samples in addition soils which had received known fluoride additions. Two soil profiles were analysed with respect to distribution with depth of soluble and labile fluoride. The equilibrium-fluoride concentration was determined after shaking the soil with a 0.01 M CaCl, solution. Isotopically exchangeable (labile) soil fluoride was determined by use of the radioactive fluorine isotope ¹⁸F. These labile fluoride values were well correlated with the amount of soil fluoride extracted by an anionexchange resin, and the latter method was consequently adopted for further determinations of labile soil fluoride. Nearly half the 1OO agricultural soil samples examined gave fluoride concentrations < 0.2 ppm in 0.01 M CaCl, extracts whereas labile fluoride values were evenly distributed around a mean of 20 ppm. For any given pH value, there appeared be an upper limit to the solubility of soil fluoride. Application to soil of superphosphate (in the field) or of fertilizer containing fluoride (in the laboratory) brought about increases in soluble soil fluoride.     

Chlorate analyses in matrices of animal origin

Sodium chlorate is being developed as a potential food-safety tool for use in the livestock industry because of its effectiveness in decreasing concentrations of certain Gram-negative pathogens in the gastrointestinal tracts of food animals. A number of studies with sodium chlorate in animals have demonstrated that concentrations of chlorate in meat, milk, wastes, and gastrointestinal contents range from parts per billion to parts per thousand, depending upon chlorate dose, matrix, and time lapse after dosing. Although a number of analytical methods exist for chlorate salts, very few were developed for use in animal-derived matrices, and none have anticipated the range of chlorate concentrations that have been observed in animal wastes and products. To meet the analytical needs of this development work, LC-MS, ion chromatographic, and colorimetric methods were developed to measure chlorate residues in a variety of matrices. The LC-MS method utilizes a Cl(18)O(3)(-) internal standard, is applicable to a variety of matrices, and provides quantitative assessment of samples from 0.050 to 2.5 ppm. Due to ion suppression, matrix-matched standard curves are appropriate when using LC-MS to measure chlorate in animal-derived matrices. A colorimetric assay based on the acid-catalyzed oxidation of o-tolidine proved valuable for measuring ≥20 ppm quantities of chlorate in blood serum and milk, but not urine, samples. Ion chromatography was useful for measuring chlorate residues in urine and in feces when chlorate concentrations exceeded 100 ppm, but no effort was made to maximize ion chromatographic sensitivity. Collectively, these methods offer the utility of measuring chlorate in a variety of animal-derived matrices over a wide range of chlorate concentrations.     

Quantitative conformation of dimethoate residues in wheat plants by single ion mass spectrometry.

A gas chromatographic-single ion mass spectrometric method was developed for determining dimethoate residues in wheat plants. The base peak (m/e 37) of dimethoate was chosen as the single ion peak, and methyl stearate was used as an internal standard for this analysis. The minimum detectable concentration of dimethoate by this method was about 0.1 ppm for a 20 g wheat plant sample. The recoveries of dimethoate were about 89% at 0.13 ppm and greater than 96% at 0.5-1 ppm.     

Diagnosing nitrogen fertilization requirements of cereals in less than 30 seconds

Abstract

Stems of barley and wheat plants of wide range in nutritional status were analysed for sap NO₃ concentration at the tillering stage using both “Merckoquant”; nitrate test strips and a specific‐ion nitrate electrode. Even though the “Merckoquanf'test strips used in this study did not give precise NO₃ readings they were found to be a satisfactory method for determining the NO₃ content of stems of cereals, and can be used in situ by farmers to predict the necessity of N fertilization for maximum grain yield. If the NO₃ sensitive area on the test strip is coloured to match the standard 500 ppm NO₃ colour in less than 30 seconds, after the application of sap, this is an indication of adequate N nutrition. If the 500 ppm NO₃ colour standard is reached between 30 to 60 seconds, then this is an indication of intermediate N nutrition and fertilization is recommended only under favorable weather conditions. If colour development of the test strip for the 500 ppm N0₃ standard takes more than 60 seconds, or the colour developed does not reach this standard, this is an indication of deficient N nutrition. Therefore, the use of the “Merchoquant”; test strips offers a useful tool in deciding if N fertilization of small‐grain cereals is needed.