Gas-liquid chromatographic-mass fragmentographic determination of low levels of diethylcarbonate in beverages.

Sodium chloride and ethanol (omitted for samples with greater than 10% alcohol) are added to the beverage sample and the sample is allowed to equilibrate in a 30 degrees C water bath. An aliquot of the headspace is injected into a gas chromatography containing a column packed with 0.2% Carbowax 1500 on 80--100 mesh Carbopack C. During the elution of diethylcarbonate (DEC), an impurity that is present in diethylpyrocarbonate, the column effluent is vented to a mass spectrometer with a multiple ion detection system and operated in the electron impact mode. The ions at m/e 63 and 91 are monitored. Lemonade, fruit drinks, wine, and beer samples (138 total) were analyzed for DEC. Sixteen samples had greater than 30 ppb DEC. Eight analyses of a lemonade sample gave a mean of 88 ppb with a coefficient of variation of 11%.     

Gas-liquid chromatographic determination of individual sugars in confectionery products.

A gas-liquid chromatographic (GLC) procedure is presented for the separation and quantitative determination of sucrose, lactose, maltose, and glucose in commercial confectionery products. By converting reducing sugars to oximes and then forming trimethylsilyl ethers of these compounds and separating them on a 6 ft X 4 mm id glass column packed with 2% OV-17 on 100--120 mesh Supelcoport, single peaks were obtained for each of the sugars. Results for sugars present in samples at levels of 5% or more are within 2.8%, on the average, of results obtained by polarization measurements. The data also compare favorably with others in the literature on similar products analyzed by other GLC procedures that do not involve oxime formation.     

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.     

太湖地区水稻最适宜施氮量研究

To determine the optimal amount of nitrogen(N) fertilizer for achieving a sustainable rice production at the Taihu Lake region of China,two-year on-farm field experiments were performed at four sites using various N application rates.The results showed that 22%-30% of the applied N was recovered in crop and 7%-31% in soils at the rates of 100-350 kg N ha 1.Nitrogen losses increased with N application rates,from 44% of the applied fertilizer N at the rate of 100 kg N ha 1 to 69% of the N applied at 350 kg N ha 1.Ammonia volatilization and apparent denitrification were the main pathways of N losses.The N application rate of 300 kg N ha 1,which is commonly used by local farmers in the study region,was found to lead to a significant reduction in economic and environmental efficiency.Considering the cost for mitigating environmental pollution and the maximum net economic income,an application rate of 100-150 kg N ha 1 would be recommended.This recommended N application rate could greatly reduce N loss from 199 kg N ha 1 occurring at the N application rate of 300 kg N ha 1 to 80-110 kg N ha 1,with the rice grain yield still reaching 7 300-8 300 kg DW ha 1 in the meantime.     

Gas chromatographic, liquid chromatographic, and titrimetric procedures for determination of glycerin in allergenic extracts and diagnostic antigens: comparative study

Three methods for the determination of glycerin are examined as applied to several allergenic extracts and diagnostic antigens. The liquid chromatographic procedure uses a sulfonic acid functional PSDVB resin (Aminex HPX-87H), a mobile phase of 0.013N H2SO4; and refractive index detection. The titrimetric procedure involves oxidation of glycerin with sodium metaperiodate followed by potentiometric titration of the resulting formic acid with sodium hydroxide. Samples are quantitated by comparing the equivalence point obtained from the sample to those obtained from a series of standards. The gas chromatographic procedure includes a column of 5% Carbowax 20 M on 80-100 mesh Chromosorb WHP; p-cresol was used as an internal standard. The 3 procedures are shown to be valid for the majority of product types examined. A positive interference was encountered in the titrimetric analysis of a tuberculin purified protein derivative that contained simple sugars. Recoveries of added glycerin ranged from 95.0 to 100.2% by the liquid chromatographic method, from 98.7 to 101.4% by the gas chromatographic method, and from 99.8 to 101.6% by the metaperiodate oxidation method when interference from simple sugars was not present. Coefficients of variation determined from 8 replicates of samples that contained glycerin were 2.2% or less for the liquid chromatographic method, 2.3% or less for the GC method, and 3.6% or less for the metaperiodate oxidation method.     

土壤碳氮对多年生能源草、覆盖作物和氮施肥的响应

Cover crop and nitrogen(N) fertilization may maintain soil organic matter under bioenergy perennial grass where removal of aboveground biomass for feedstock to produce cellulosic ethanol can reduce soil quality. We evaluated the effects of cover crops and N fertilization rates on soil organic carbon(C)(SOC), total N(STN), ammonium N(NH_4-N), and nitrate N(NO_3-N) contents at the0–5, 5–15, and 15–30 cm depths under perennial bioenergy grass from 2010 to 2014 in the southeastern USA. Treatments included unbalanced combinations of perennial bioenergy grass, energy cane(Saccharum spontaneum L.) or elephant grass(Pennisetum purpureum Schumach.), cover crop, crimson clover(Trifolium incarnatum L.), and N fertilization rates(0, 100, and 200 kg N ha~(-1)). Cover crop biomass and C and N contents were greater in the treatment of energy cane with cover crop and 100 kg N ha~(-1) than in the treatment of energy cane and elephant grass. The SOC and STN contents at 0–5 and 5–15 cm were 9%–20% greater in the treatments of elephant grass with cover crop and with or without 100 kg N ha~(-1)than in most of the other treatments. The soil NO_3-N content at 0–5 cm was 31%–45% greater in the treatment of energy cane with cover crop and 100 kg N ha~(-1)than in most of the other treatments.The SOC sequestration increased from 0.1 to 1.0 Mg C ha~(-1)year~(-1)and the STN sequestration from 0.03 to 0.11 Mg N ha~(-1)year~(-1)from 2010 to 2014 for various treatments and depths. In contrast, the soil NH_4-N and NO_3-N contents varied among treatments,depths, and years. Soil C and N storages can be enriched and residual NO_3-N content can be reduced by using elephant grass with cover crop and with or without N fertilization at a moderate rate.     

Gas-liquid chromatographic determination of nitrate and nitrite in cheese, ham, fish sausage, cod roes, and salmon roes

The 2,4-xylenol method was modified and a gas-liquid chromatographic (GLC) method was developed for nitrate and nitrite determinations in several foods. Either a flame ionization (FID) or an electron capture detector (ECD) can be used. Proteins and fats are removed from warm alkaline water with zinc sulfate and filtered. The filtrate is evaporated to dryness, redissolved in water, and reacted with 2,4-xylenol in the presence of sulfuric acid to form 6-nitro-2,4-xylenol. Interfering chlorides are precipitated with silver sulfate and the nitrosylenol is extracted with hexane, concentrated, and injected. Nitrite in the filtrate is distilled at pH 5, collected in alkaline solution, and dried. The residue is oxidized to nitrate with permanganate in the presence of sulfuric acid, and then chromatographed in the same manner as nitrate. Recoveries from several foods were 83--100% for nitrate and 80--100% for nitrite. The limit of sensitivity was 0.1 ppm for both residues.     

Gas-liquid chromatographic determination of nikethamide in injectable preparations.

A gas-liquid chromatographic (GLC) method, using a 4% XE-60 on 80-100 mesh Gas-Chrom Q column, a flame ionization detector, and anthracene as the internal standard, has been developed for the direct determination of nikethamide. Eight collaborators analyzed 4 samples, using methanol as the solvent; the coefficients of variation obtained ranged from 1.19 to 3.20%. In a limited study with acetone as the solvent, the coefficients of variation ranged from 0.59 to 1.96%. The GLC method with acetone as a solvent has been adopted as official first action.     

不同制粉方式对运黑161全麦粉加工特性的影响

为探讨不同制粉方式及不同粒度对黑小麦流变学特性及加工品质的影响,将运黑161黑小麦经直接粉碎法和回添法制得的全麦粉分别过80、100、120目筛,以运黑161黑小麦面粉为对照,分析全麦粉淀粉含量、水合特性、发酵特性以及流变学特性。结果表明,直接粉碎且过80目筛的全麦粉支链淀粉含量最高,为80.18%,破损淀粉含量最低,为9.93%,溶解度、膨润力最小,分别为2.5%和3%。回添法制备的全麦粉面团发酵高度、持气率小于直接粉碎法。直接粉碎且过80目筛全麦粉的粉质质量指数最高,为59.5,形成时间和稳定时间分别为3.45和3.2 min,较接近于黑小麦面粉,且该全麦粉的阻力值、最大阻力值在醒发时间135 min时最大,用该全麦粉制作的面包感官得分最高。综上,以直接粉碎且过80目筛制备的全麦粉为原料制作的全麦面包品质较好。本研究结果为黑小麦全麦面包研发提供了理论基础。     

Simple analytical method for organophosphorus pesticide determination in unpolished rice, using removal of fats by zinc acetate

A rapid and simple method is developed for the determination of organophosphorus pesticides in unpolished rice. The new method incorporated acetonitrile-water (1 + 1) extraction, removal of fats by zinc acetate, and further cleanup on an activated charcoal chromatographic column. The higher fatty acids in the extract react rapidly with zinc acetate to form insoluble zinc carboxylates, which precipitate. Additional interferences were cleaned up on an activated charcoal chromatographic column, and organophosphorus pesticides adsorbed on the activated charcoal were eluted with acetone-hexane. Dimethoate is not retained on the activated charcoal and must be extracted with dichloromethane from the first acetonitrile-water eluate. Pesticides are measured by flame photometric gas chromatography. Recoveries from 50 g unpolished rice samples fortified with 5-50 micrograms diazinon, 6-30 micrograms parathion, 8-40 micrograms fenitrothion and IBP, 10-50 micrograms dimethoate and fenthoate, 20-100 micrograms malathion, or 40-200 micrograms EPN ranged from 75.7 to 95.8%.     

Gas chromatographic determination of ametryn and its metabolites in tropical root crops

Residue analysis of the herbicide ametryn (2-methylthio-4-ethylamino-6-isopropylamino-s-triazine) is widely known but an analytical method for determining its metabolites has not yet been reported in the literature. A method has been developed for the extraction and determination of ametryn and 3 metabolites, 2-methylthio-4-amino-6-isopropylamino-s-triazine (GS-11354), 2-methylthio-4,6-diamino-s-triazine (GS-26831), and 2-methylthio-4-amino-6-ethylamino-s-triazine (GS-11355) in taniers , yams , cassava. Residues were extracted from crops with ethyl acetate-toluene (3 + 1 v/v), using a Polytron homogenizer and anhydrous sodium sulfate added for drying. The extracts were cleaned up by automated gel permeation chromatography on Bio-Beads SX-3 gel in the same solvent system. Quantitative determination was performed by gas chromatographic (GC) analysis on a column packed with 5% DEGS -PS on 100-120 mesh Supelcoport using either an N-P detector or a flame photometric detector ( FPD ) in the sulfur mode. Minimum detection by the flame photometric detector is 10 ng each for ametryn , GS-11354, and GS-11355 and 21 ng for GS-26831; by the N-P detector, 0.3 ng of each component gives easily quantitatable peaks. On a parts per million basis, starting with 25 g sample, the FPD detected a minimum level of 0.04 microgram/g each for ametryn , GS-11354, and GS-11355, and 0.08 microgram/g for GS-26831. The N-P detector could detect 0.0024 microgram/g for all 4 compounds. In addition to superior sensitivity, instrumental conditions allowed the complete separation of components in 10 min, for the N-P detector; more than 30 min was required for the FPD . Recoveries from fortified crops ranged from 67 to 111% at levels of 0.1-1.0 microgram/g.     

Determination of novobiocin residues in milk, blood, and tissues by liquid chromatography

Residues of novobiocin in milk, blood, and tissues can be detected by microbiological tests but cannot be distinguished from other antibiotics. A simple liquid chromatographic (LC) method was developed for identification of residues. Tissues were blended and milk and blood serum were mixed with 0.2M NH4H2PO4. The mixture was deproteinized by adding aqueous methanol and filtering. The LC apparatus consisted of a variable wavelength detector, set at 340 nm, an automatic loop injector, and a C18 column with guard cartridge. The flow rate was 1 mL/min and the solvent mixture of 0.01M H3PO4-acetonitrile-methanol was programmed from 50 + 0 + 50 (0-1 min) to 20 + 80 + 0 (20 min). Novobiocin was concentrated directly by solid-phase extraction on the analytical column. Five or more 200 microL aliquots of the filtrate in water-methanol (1 + 1) (adjusted if necessary) were injected with the column solvent at 50 + 0 + 50. After the final injection, the program was run to completion. Recoveries were 90-100% with sensitivities of 0.05 ppm or less. The procedure should be adaptable for use with formulations and feeds.     

Determination of vitamin D3 in liquid multivitamin preparation, using reverse phase, solid phase extraction liquid chromatography

A method is described for the determination of vitamin D3 in a liquid multivitamin preparation by liquid chromatography. Samples are purified on a disposable reverse phase extraction (SPE) column with a mobile phase of methanol-2-propanol (97 + 3) and are analyzed on a Zorbax ODS (5 micron) column with an acetonitrile-2-propanol-water (90 + 8 + 2) solvent system. Vitamin D3 is completely resolved from other interfering compounds within approximately 21 min and is detected with a UV detector at 254 nm. A mean of 98.5% of theory with a coefficient of variation of 3.8% was found for determination of vitamin D3 in a commercial preparation.     

Improved cleanup for gas chromatographic determination of propiconazole residues in soil, wheat grain, straw, and leaves

A simple and sensitive method is described for determination of propiconazole, a new type of broad-spectrum systemic fungicide, in soil, wheat grain, straw, and leaves. Pesticide residues in or on grain and green plant materials are extracted with methanol (or a mixture of methanol and water (4 + 1), for soil), partitioned into methylene chloride, and cleaned up on an alumina column for grain and soil or an activated charcoal column for green plant materials. The amount of residue is quantitatively measured by gas chromatography using an alkali flame ionization detector in the nitrogen-sensitive mode. Recoveries from soil, grain, and green plant materials fortified at 0.1-5 mg/kg are better than 80%. The practical detection limits of this method are 0.01 mg/kg in grain and soil and 0.02 mg/kg in green plant materials.     

Gas chromatographic determination of mecarbam and its metabolites mecarboxon, diethoate, and diethoxon in cottonseeds

A gas chromatographic method is described for determining residues of mecarbam and 3 of its metabolites, mecarboxon, diethoate, and diethoxon, in cottonseeds. For mecarbam analysis, following Soxhlet extraction with chloroform (after blending), the oily extract is partitioned with propylene carbonate and cleaned up on a silica gel column. Metabolites are extracted by the same method, followed by cleanup of mecarboxon on a silica gel column or diethoxon on an alumina column; cleanup of diethoate can be performed on either column. All 4 compounds are determined using a flame photometric detector equipped with a phosphorus filter. Average recoveries for cottonseed samples fortified with 0.03-1.0 ppm mecarbam ranged from 80 to 88%. Average recoveries were 81-88% for mecarboxon and 90-92% for diethoate (alumina column) and diethoxon from samples fortified with 0.05-1.0 ppm. Average recovery of diethoate from samples cleaned up on the silica gel column were 84-88% in the range of 0.05-0.2 ppm. Values obtained for mecarbam residues in field-treated samples are also presented.     

High pressure liquid chromatographic detection and estimation of furazolidone and nitrofurazone in animal feeds.

The feed sample is extracted with acetone or dimethylformamide-acetone (1 + 1) and the filtered extracts are evaporated to dryness. The residue is dissolved in chloroform and transferred to a silica gel column. The nitrofurans are eluted with methanol-chloroform (50 + 50). A portion of the eluate is evaporated to dryness and the residue is redissolved in a small volume of methanol. Aliquots of the methanolic solution are injected into a liquid chromatograph with a muBondapak C18 column, using 30% acetonitrile as the eluting solvent and ultraviolet detection at 365 nm. Several samples spiked with 0.5--50 ppm furazolidone or nitrofurazone and 2 commercial samples were analyzed by the proposed method.     

Gas chromatographic determination of alachlor in microencapsulated formulations: mini-collaborative study

An isothermal gas chromatographic method for measuring alachlor in Micro-Tech (microencapsulated) formulations was tested by 5 collaborators. The samples were prepared in acetone, and alachlor was determined using a gas chromatographic column of 10% SP-2250 on 100-120 mesh Supelcoport. Di-n-pentylphthalate was used as the internal standard. Collaborators made single determinations on 5 samples distributed as blind duplicates. The mini-collaborative study generated 47 data points. The coefficient of variation (CVo-pooled) was 1.35%, and CVx-pooled was 0.73%. The method was simple to use and did not reveal any interferences in samples tested. The method has been adopted official first action as an AOAC-CIPAC method.     

黑土肥料长期定位试验冻土分割搬迁后土壤融合效果评价

为了明确黑土长期定位试验土壤搬迁后与新址的融合效果,以一个搬迁土块为研究对象,明确搬迁土块间的接缝处土壤与距接缝处不同距离的中心土壤在理化特性上的不同。结果表明,0~20 cm层次土体中心50 cm处的田间持水量比接缝处高5%,容重低4%,变异系数均明显高于其他层次;20~40 cm层次,土壤的固相率和容重高于其他层次,田间持水量降低,土块横切面各部位物理性质均无明显差别;剖面底部80~100 cm层次接缝处土壤松散缝处的固相率比30 cm和土体中心处低4.3%,液相率低3.1%,气相率高出7.6%,容重下降8.3%。0~40 cm土层的缝处、距缝30 cm和距缝50 cm处的孔隙率均低于40~100 cm层次,其中80~100 cm层次的孔隙率最大,20~40cm孔隙率最低为44.2%;土壤饱和导水率0~20 cm层次为35.3~38.0 cm/d,随着深度的加深呈下降趋势,均小于20cm/d;而80~100 cm层次缝处的饱和导水率值高达144.4 cm/d,是表层土壤的4倍。同一层次搬迁土块缝处与土块中心土壤速效养分无明显差别,缝处全氮含量均高于土块的其他位置,且与距缝30 cm和50 cm处的数值差异均达到显著水平(P0.05);pH随着土层的加深逐渐增大,碱解氮和土壤有机碳含量随着土层的加深而下降。长期定位土壤搬迁5 a后,深层土壤接缝处还处于疏松状态,下层土壤的融合要弱于上层土壤。     

覆膜和施肥对玉米产量和土壤温度、硝态氮分布的影响

【目的】采用垄沟覆膜栽培技术,研究了西北黄土塬区不同施肥及覆膜处理对玉米(Zea mays L.)产量、土壤温度和土壤硝态氮分布的影响,为粮食安全和农业可持续发展提供依据。【方法】研究采用覆膜和施肥田间试验,小区试验设置了6个处理,1)对照不覆膜,不施肥;2)覆膜不施肥;3)不覆膜基施N 80 kg/hm2、P2O580kg/hm2,无追肥;4)覆膜基施纯N 80 kg/hm2、P2O580 kg/hm2,无追肥;5)不覆膜基施N 80 kg/hm2、P2O580kg/hm2,追施N 80 kg/hm2;6)覆膜基施N 80 kg/hm2、P2O580 kg/hm2,追施N 80 kg/hm2。【结果】1)覆膜对前期土壤温度的影响大于后期,在7月前,覆膜处理0—20 cm土壤温度平均增加2.3℃,对玉米的发芽和早期生长有良好的促进作用,7月后,覆膜处理对土壤温度增加的平均值为1.2℃。在6月中旬以前,施肥处理的土壤温度略高于不施肥处理;6月中旬以后差异减小,施肥处理对土壤温度的影响不明显。2)播种后一个月,施肥处理土壤硝态氮主要聚集在0—30 cm土层,以主根为中心,纵向近似对称分布,在根系下方40 cm处,形成一个孤岛,施肥处理是不施肥处理的1.65倍;播种后两个月,表层土壤硝态氮含量下降至30.77~48.67 mg/kg。覆膜处理在施肥初期有减缓硝态氮向下层迁移速度的作用,影响范围为0—80 cm深。3)水分利用效率(WUE)与施肥量呈正相关,最高为2.09 kg/m3。在相同施肥处理下,覆膜明显提高WUE,施基肥处理,覆膜比不覆膜的WUE提高12.8%~19.5%;施基肥和追肥处理,覆膜比不覆膜的WUE提高20.3%~27.4%。4)百粒重、穗粒重与产量呈正相关关系,产量提高是百粒重和穗粒重增加的直接结果,施肥和覆膜对百粒重和穗粒重的提高效果明显。覆膜在施肥处理下的增产效果显著,连续三年,施基肥处理下,覆膜处理增产10.61%、9.48%和15.36%;施基肥和追肥处理下,覆膜增产16.61%、20.94%和12.24%。【结论】施肥和覆膜处理比不施肥不覆膜处理产量增加23.42%~83.23%。综合考虑覆膜和施肥对土壤温度、土壤硝态氮含量和水分利用效率的影响,本试验推荐采用垄沟覆膜栽培技术,氮肥基肥和追肥各施N 80 kg/hm2。     

Simplified method for determining polychlorinated biphenyls, phthalates, and hexachlorocyclohexanes in air

A simplified method for determining polychlorinated biphenyls (PCBs), phthalates, and benzene hexachlorides (BHCs) in air has been developed. Florisil is used as the adsorbent, and compounds are eluted by liquid chromatography with 10% 2-propanol in hexane. PCBs are separated from phthalates plus BHCs on a cyanopropyl column with a gradient containing 10% 2-propanol in hexane and 100% hexane as the mobile phase. Two fractions are collected: one contains PCBs and the other contains phthalates plus BHCs, which are then determined by gas chromatography using a 63Ni electron-capture detector and a DB-5-bonded, fused-silica capillary column.