Improved cleanup and derivatization for gas chromatographic determination of monosodium glutamate in foods

A gas chromatographic procedure is described for determining monosodium glutamate (MSG) in several types of food. A sample is extracted with acetone-water (1 + 1). Acetone is evaporated and an aliquot of the extract is buffered with 1M NH4OH-1M NH4Cl pH 9 solution, and chromatographed directly on a column of QAE Sephadex A-25 that has been pretreated with the same buffer. MSG is eluted with 0.1N HCl, and a portion of the eluate is evaporated to dryness and reacted with dimethylformamide(DMF)-dimethylacetal to form the glutamic acid derivative, which is injected into a gas chromatograph and measured by flame ionization detection. Recoveries of MSG from sample fortified at 5-500 mg ranged from 92.8 to 100%.     

Simplified cleanup and liquid chromatographic determination of oxamyl residues in potato tubers

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of oxamyl residues in potato tubers. Samples are extracted with methanol, partitioned into dichloromethane, and cleaned up using Sep-Pak Florisil cartridges. LC determination is performed using a Zorbax PSM 60 size exclusion column with an acetonitrile-water (1 + 9) mobile phase and UV detection at 254 nm. Recovery of oxamyl from spiked control tubers averaged 94.1 and 85.9% at fortification levels of 0.4 and 0.08 micrograms oxamyl/g tuber, respectively. The minimum detectable concentration of oxamyl by this method is 0.01 micrograms/g.     

Simplified cleanup and gas chromatographic determination of organophosphorus pesticides in crops

A simple and efficient cleanup method for gas chromatographic determination of 23 organophosphorus pesticides in crops including onion is described. The sample was extracted with acetone. The extract was purified with coagulating solution, which contained ammonium chloride and phosphoric acid, and then filtered by suction. The filtrate was diluted with NaCl solution and reextracted with benzene. The organic layer was evaporated and injected into a gas chromatograph equipped with a flame photometric detector (FPD) and fused silica capillary columns (0.53 mm id) coated with silicone equivalent to OV-1701, OV-1, and SE-52. Onion extract, which contained FPD interferences, was cleaned up on a disposable silica cartridge. Recoveries of most organophosphorus pesticides from spiked crops: mandarin orange, tomato, spinach, sweet pepper, broccoli, lettuce, and onion at levels of 0.02-0.28 ppm, exceeded 80%, but the water-soluble pesticides dichlorvos and dimethoate gave poor recoveries in all crops; the nonpolar pesticides disulfoton, chlorpyrifos, fenthion, prothiophos, and leptophos were not recovered quantitatively in spinach, sweet pepper, broccoli, and lettuce. IBP, edifenphos, phosmet, and pyridaphenthion were not recovered from onion because of adsorption to the silica cartridge. The detection limits ranged from 1.25 to 17.5 ppb on a crop basis.     

Ion-pair extraction cleanup for liquid chromatographic determination of bentazon in crops and soil

Bentazon was selectively extracted as an ion pair with tetrabutylammonium ion into dichloromethane. This technique was used to clean up crop and soil samples before determination of bentazon by reverse phase liquid chromatography and UV detection. Recoveries from potatoes, cucumbers, wheat grain, and clay soil were 77-103%, with a detection limit of 0.02 mg/kg.     

Improved gas chromatographic method for quantitation of deoxynivalenol in wheat, corn, and feed

A gas chromatographic (GC) method is described to determine deoxynivalenol in wheat and corn at levels as low as 20 ppb. Ground samples are extracted with water, adsorbed onto a Clin Elut column, extracted with ethyl acetate, and passed through a silica gel Sep-Pak cartridge. The final extract is then derivatized with N-heptafluorobutyrylimidazole and quantitated by GC using an electron capture detector. Recoveries are greater than 85% for spiked samples at levels of 50-1000 ppb. Results for wheat, corn, and mixed feed samples are given as well as the results of an interlaboratory study on a naturally contaminated wheat sample.     

Rice straw biochar amended soil improves wheat productivity and accumulated phosphorus in grain

Abstract

Biochar is a pyrolyzed biomass produced under limited oxygen or oxygen absent conditions. Few investigations have been conducted to determine the combined effect of biochar with chemical fertilizer on growth, yield and nutrient distribution pattern in root, shoot and grain in wheat as well as changes in soil physiochemical properties. This research was designed to study the combined effect of chemical fertilizer and rice straw-derived biochar on soil physio-chemical properties, growth, yield and nutrient distribution pattern within wheat plant tissue and grain. Results showed that rice straw biochar caused a significant decrease in soil pH and increase in soil organic matter as well as nutrients like total nitrogen (TN), potassium (K), magnesium (Mg) and boron (B) due to incubation. Result also showed that root biomass and straw did not differ between Bangladesh Agricultural Research Council (BARC) and ½ BARC?+?rice straw biochar treatment. Similarly, thousand grain weight and grain yield did not differ between the same treatments. The phosphorus concentration in wheat grain was highest in ½ BARC?+?rice straw biochar as compared to other treatments. The use of rice straw biochar in addition to the chemical fertilizers in wheat production systems is an economically feasible and practical nutrient management practice. Our findings urged that reduction of chemical fertilizer application is possible with supplementation of rice straw biochar.     

Frequent addition of wheat straw residues to soil enhances carbon mineralization rate

In many ecosystems, residues are added frequently to soil, in the form of root turnover and litter fall. However, in most studies on residue decomposition, residues are added once and there are few studies that have investigated the effect of frequent residue addition on C mineralization and N dynamics. To close this knowledge gap, we mixed mature wheat residue (C/N 122) into soil at a total rate of 2% w/w once at the start (R1×), every 16 days (R4×), every 8 days (R8×) or every 4 days (R16×). Un-amended soil served as control. All treatments were mixed every 4 days. Soil respiration was measured continuously over the 80-day incubation. Inorganic N, K₂SO₄-extractable C and N, chloroform-labile C and N (as an estimate of microbial biomass C and N), soil pH and microbial community composition were assessed every 16 days. Increasing frequency of residue addition increased C mineralization per g residue. Compared to R1×, cumulative respiration per g residue at the end of the incubation (day 80) was increased by 57, 82 and 92% in R4×, R8× and R16×, respectively. The largest differences in soil respiration per g residue occurred in the first 30 days. Despite large increases in cumulative respiration, frequent residue addition did not affect inorganic N or K₂SO₄-extractable N concentrations, chloroform-labile C and N or soil pH. Compared to the control, all residue treatments resulted in increases in chloroform-labile C and N and soil pH but decreased inorganic and K₂SO₄-extractable N. Microbial community composition was affected by residue addition, however there were no consistent differences among residue treatments. It is concluded that experiments with single residue additions may underestimate residue decomposition rates in the field. The increased C mineralization caused by frequent residue additions does not appear to be due to an increased microbial biomass or changes in microbial community composition, but rather to increased C mineralization per unit biomass.     

Optimized gel permeation chromatographic cleanup for soil, sediment, wastes, and oily waste extracts for determination of semivolatile organic pollutants and PCBs

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).     

秸秆颗粒还田对土壤养分和冬小麦产量的影响

为明确秸秆颗粒还田在农业生产中推广应用的可行性,在山东省冬小麦-夏玉米一年两熟种植区通过田间微区试验,研究了秸秆不还田(CK)、常规粉碎还田(CCSI)和秸秆颗粒还田(GSI)对耕层土壤养分含量、冬小麦群体茎蘖数、旗叶净光合速率、叶绿素含量、干物质积累及分配和小麦产量的影响。结果表明:与CK和CCSI处理相比,GSI处理显著提高土壤有机质、碱解氮和有效磷的含量;增加基本苗和分蘖成穗率,显著提高有效穂数13.23%和16.64%。同时,GSI处理显著提高灌浆期叶面积指数、旗叶叶绿素含量和净光合速率,改善开花后旗叶光合性能,促进地上部干物质积累及其向籽粒的转运。与CK和CCSI处理相比,GSI处理的开花后干物质向籽粒的转运量显著提高19.65%和14.75%,籽粒产量显著提高9.69%和10.71%。相关分析表明,穗粒数和千粒重对产量影响不显著,有效穂数的提高是秸秆颗粒还田增产的主要原因。因此,秸秆颗粒还田可作为一种安全有效的还田方式,在农业生产中推广应用。     

Improved cleanup technique for the estimation of endosulfan and endrin residues.

An improved cleanup technique has been developed for the extraction of endosulfan and endrin from crops. The technique involves the use of Nuchar C-190N as adsorbent and a mixture of n-hexane and acetone (4+1) as the eluting solvent. The mean percentage recoveries of endosulfan (I and II) and endrin from plant tissue extracts fortified at levels of 0.5-2.0 ppm varied from 86 to 102 and 97 to 100, respectively.     

Rapid gas chromatographic determination of ethylene oxide, ethylene chlorohydrin, and ethylene glycol residues in rubber catheters

Isothermal gas chromatography with flame ionization detection was used to determine residual ethylene oxide (EtO), ethylene chlorohydrin, and ethylene glycol in soft rubber catheters that had been sterilized with EtO. Catheter samples were extracted by shaking with carbon disulfide, and the extract was analyzed on a 3% Carbowax 20M on 80-100 mesh Chromosorb 101 column, using nitrogen as the carrier gas. Ten replicate injections of a mixed standards solution gave coefficients of variation of 1.91, 1.23, and 4.74% for EtO, ethylene chlorohydrin, and ethylene glycol, respectively. A linear response was obtained with concentrations ranging from 1.0 to 7.9 micrograms EtO, 14.0 to 88.0 micrograms ethylene chlorohydrin, and 31.0 to 98.5 micrograms ethylene glycol. The proposed method detected as little as 0.5, 5.0, and 16.5 ng EtO, ethylene chlorohydrin, and ethylene glycol, respectively.     

Gas chromatographic determination of electron capture sensitive volatile industrial chemical residues in foods, using AOAC pesticide multiresidue extraction and cleanup procedures

Electron capture (EC) gas chromatographic (GC) parameters have been developed for determining some of the more volatile industrial chemicals that can be determined by the AOAC multiresidue method for organochlorine and organophosphorus pesticides with modified GC operating conditions. Retention times relative to pentachlorobenzene are reported for 143 industrial chemicals, pesticides, and related compounds on OV-101 GC columns at 130 degrees C. Also reported for most of the compounds are recoveries from fortified samples carried through the AOAC extraction and cleanup procedures for fatty and/or nonfatty foods, Florisil elution characteristics, and GC relative retention times on mixed OV-101 + OV-210 columns at 130 degrees C. Our laboratory has used the modified EC/GC parameters with the AOAC multiresidue extraction/cleanup procedures to determine many volatile halogenated industrial chemical contaminants in foods, chiefly in samples of fresh-water fish. Other modifications of the AOAC method are described to improve the tentative identification and quantitative measurement of these volatile residues.     

Gas chromatographic determination of deoxynivalenol in wheat

Modifications to a published method are described for the determination of deoxynivalenol (DON) in wheat by gas chromatography with electron capture quantitation of the heptafluorobutyrate derivative. In the modified method, DON is extracted by shaking the sample with methanol-water on a wrist-action shaker, followed by filtration through rapid flow paper. One concentration step is eliminated, and a hexane wash is incorporated to remove toluene from the silica gel column. Recoveries of DON from wheat samples spiked at 0.1, 0.5, and 1.0 ppm ranged from 77.3 to 86.3% and averaged 81.5%.     

小麦籽粒中微量铅的快速测定技术(简报)

为建立一种快速测定粮食中微量铅的新方法,以南阳彩色小麦为材料,用微波压力消解技术快速处理样品,对测定条件进行优化,并与国家颁布标准方法(GB/T5009.12-2003)进行比较。结果表明:加标回收率为92.5%～96.8%,相对标准偏差RSD(Relative Standard Deviation)为0.67%～1.7%(n=11),铅的最低检出限为0.0099mg/L,测定的线性范围为0.850～206.0mg/L,相关系数为0.996,电极斜率为24.160。样品用该法与国标方法对照测定并进行显著性检验证明,该方法具有直观、快速、简便、灵敏、准确、适于现场进行测定的显著优点。     

Liquid chromatographic determination of cephapirin residues in milk

A liquid chromatographic (LC) method was developed for quantitative determination of cephapirin residues in milk that also resolved cephapirin from ampicillin, cloxacillin, and penicillin G. Diluted milk was passed through a C18 cartridge on which the cephapirin was adsorbed; then, interfering material was removed by washing with water and methylene chloride and cephapirin residues were eluted with methanol-acetonitrile (25 + 75). After drying, residues were dissolved in the mobile phase for injection. The LC system had an ultrasphere-ODS column with RP-18 Spheri-10 guard column and a UV detector with a 254 nm filter. The mobile phase was 85% sodium acetate (0.01M) and 15% methanol-acetonitrile (25 + 75) with a flow rate of 1 mL/min. Sensitivity was 20 ppb or less with a recovery of 61-80% in the range studied. Other beta-lactam antibiotics tested did not interfere with detection of cephapirin. Analysis of 30 samples of commercial homogenized milk obtained for a survey of antibiotics in consumer milk in Canada revealed no detectable cephapirin residues.