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1.
气相色谱最优化分离多种有机磷农药 总被引:1,自引:0,他引:1
引 言 多种有机磷农药的色谱分离,一直是农药残留分析的重要方面,我们利用气相色谱FPD检测器,根据R.J.Laub等提出的气相色谱窗图最优化方法,选择较好的窗图,对12种有机磷农药进行了分离,发现当用86%的4%DC-200Chromosorb W.HP100—120目加14%的4%QF-1ChromosorbW.HP 100—120目的固定相机械混合时,对12种有机磷农药的难分离物质对,可提高其分离度或达到完全分离。 相似文献
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高分子多孔微球富集-HPLC法测定水体中的有机磷 总被引:1,自引:0,他引:1
本文提出应用国产高分子多孔微球-GDX系列富集-反相高效液相色谱法测定废水中久效磷、乐果、甲基对硫磷三种有机磷农药分析方法。三种不同型号色谱固定相(GDX-102,GDX-301和GDX-501)对水体中ng/mL级久效磷、乐果和甲基对硫磷的富集效率分别达到85%、82%和93%以上。采用μ-BondapakC18作固定相,以60%甲醇水溶液作流动相,对三种有机磷农药的分离度可达到1.2以上。本法用于分析水体中有机磷农药,结果令人满意。 相似文献
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高分子多孔微球富集—HPLC法测定水体中的有机磷 总被引:1,自引:0,他引:1
本文提出应用国产高分子多孔微球-GDX系列富集-反相高效液相色谱法测定废水中久效磷、乐果、甲基对硫磷三种有机磷农药分析方法。三种不同型号色谱固定相(GDX-102,GDX-301和GDX-501)对水体中ng/mL级久效磷、乐果和甲基以硫磷的富集效率分别达到85%、82%和93%以上,采用μ-Bondapak C18作固定相,以60%甲醇水溶液作流动相,对三种有机磷农药的分离度可达到1.2以上。本 相似文献
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毛细管气相色谱法测定牛奶中有机氯和有机磷农药残留量 总被引:18,自引:0,他引:18
采用一个较快速、简单的方法测定牛血中有机氯和有机磷农药残留物。牛奶中农残经氯仿萃取和固相提取净化后,分别用气相色谱-电子捕获检测器和气相色谱-火焰光度检测器直接测定,色谱柱为HP-1接HP-5、DB17大口径石英毛细管柱。本法对17种有机氯农残的回收效率范围为71.2% ̄99.7%,检测限为0.5 ̄9μg/kg。而11种有机磷农残的回收率范围为70.1% ̄96.1%,检测限则为0.01 ̄0.04m 相似文献
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建立超声波辅助萃取-气相色谱法同时分离测定蔬菜中5种有机磷农药残留量的:弓.法。实验结果表明,采用超声波加速提取有机磷农药残留,样品提取效果好,干扰物少,检测快速;在DB-1701色谱柱中,供试的5种有机磷农药分离良好;以FPD为检测器,选择性较好。方法的检出限为0.004-0.01μg/mL,5种农药在2个添加水平下的回收率为78.9%-105.9%,测定结果的相对标准偏差为2.6%-7.6%(n=6)。该方法具有测定有机磷农药种类多、快速等优点,能满足农药多残留分析的要求。 相似文献
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超声辅助固相萃取/离子阱气相色谱-质谱联用测定蔬菜中有机磷农药残留 总被引:1,自引:0,他引:1
通过超声辅助固相萃取提取并富集蔬菜中残留的乐果和氧化乐果等9种有机磷农药,采用离子阱二级质谱定性并定量检测其含量,建立了气相色谱-质谱联用测定蔬菜中有机磷农药残留的分析方法.结果表明,所建立的方法简单,快速,灵敏度高.9种有机磷农药的检出限为0.02~0.04 μg/mL,添加回收率为75.07%~99.47%. 相似文献
10.
气相色谱-质谱法快速筛选测定浓缩苹果汁中105种农药残留量 总被引:24,自引:9,他引:24
采用硅藻土柱层析法对样品中的农药进行提取及净化后,用气相色谱—质谱法在选择离子监测模式下进行快速测定,以保留时间和特征离子定性定量;采用此方法测定了包括有机氯农药、有机磷农药、氨基甲酸酯农药、拟除虫菊酯农药、三嗪类农药在内的105种农药,大多数农药的线性范围为0.05~10mg/kg,相关系数大于0.99;90%以上农药在0.2mg/kg添加水平的平均回收率在70%~110%的范围内。 相似文献
11.
Speciation analysis of arsenic compounds in edible oil by ion chromatography-inductively coupled plasma mass spectrometry 总被引:1,自引:0,他引:1
An inductively coupled plasma mass spectrometer (ICP-MS) was used as an ion chromatographic (IC) detector for the speciation analysis of arsenic in edible oil. The arsenic species studied include arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine and arsenocholine. Gradient elution using (NH(4))(2)CO(3) and methanol at pH 8.5 allowed the chromatographic separation of all species in less than 8 min. Effluents from the IC column were delivered to the nebulizer of ICP-MS for the determination of arsenic. The concentrations of arsenic species have been determined in several used and fresh vegetable oil samples. In this study, a microwave-assisted extraction method was used for the extraction of arsenic species from oil samples. The extraction efficiency was better than 92% and the recoveries from spiked samples were in the range of 90-105%. The precision between sample replicates was better than 8% for all determinations. The limits of detection were in the range of 0.008-0.024 ng mL(-1) for various arsenic species based on peak height, which corresponded to 0.08-0.24 ng g(-1) in the original oil sample. The major arsenic species in the used oil samples varied based on the food items cooked. 相似文献
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Micellar electrokinetic capillary chromatography (MEKC) with laser-induced fluorescence detection is used for the analysis of three classes of aminophospholipids: phosphatidylethanolamine (PE), phosphatidylserine (PS), and lysophosphatidylethanolamine (LPE) molecular species. 3-(2-Furoyl) quinoline-2-carboxaldehyde (FQ), a fluorogenic dye, was employed for labeling of these phospholipids. The FQ-labeled lipid species were then separated by sodium deoxycholate MEKC modified with methyl-beta-cyclodextrin. Baseline resolution of each class of phospholipids was achieved within 7 min. The migration time in each class increased with the carbon number of their side aliphatic chain. Separation efficiencies of approximately 3x10(5) plates were observed for most of these species. Concentration detection limits (3 sigma) were from 10(-9) to 10(-10) M for PE and LPE species and from 10(-8) to 10(-9) M for PS species. The relative standard deviations for migration time and peak area were less than 0.9% and 4.5%, respectively, for seven PE species. This method was applied to the separation of PE isolated from HT29 human colon cancer cells and roughly 30 PE species were resolved. 相似文献
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A new version of the direct injection nebulizer (DIN) is used to interface liquid chromatographic (LC) separations with element-selective detection using inductively coupled plasma mass spectrometry (ICP-MS). The DIN injects all of the sample into the ICP and has a dead volume of less than 1 microliter. Charged species of arsenic and tin are separated as ion pairs on a micro-scale (1 mm i.d.), packed, reversed-phase column. Detection limits are 0.2-0.6 pg for arsenic and 8-10 pg for tin. For methanol + water eluents, the signal is highest at 25% methanol and stays within 25% of this maximum as the methanol fraction is varied from 20 to 80%. Compared with LC-ICP-MS with conventional nebulizers, the absolute detection limits and chromatographic resolution are substantially superior, and the dependence of analyte signal on solvent composition is somewhat less severe with the DIN. 相似文献
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水相中丁基锡化合物同时衍生/萃取气相色谱/火焰光度检测方法研究 总被引:2,自引:0,他引:2
本文建立了水相中丁基锡化合物的衍生/萃取一步进行气相色谱/火焰光度检测的方法,探讨了溶剂,氮气流速,温度及火焰条件对分离及测定的影响,获得了理想的分离及检测条件。检出限分别为一丁基锡(MBT)及二丁基锡(DBT)0.25ng,三丁基锡(TBT)及四丁基锡(Bu4Sn)0.5ng;线性范围0-8ng,相对标准偏差小于4%。 相似文献
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Simultaneous determination of retinol, alpha-tocopherol and beta-carotene in serum by isocratic high-performance liquid chromatography. 总被引:3,自引:0,他引:3
A simultaneous determination of retinol, alpha-tocopherol and beta-carotene in serum by high-performance liquid chromatography is described. Total analysis time is 13 min. A reversed-phase (Ultrasphere ODS, 5 microns) column is used with a mobile phase of acetonitrile-methanol-dichloromethane (70:10:20, v/v/v) and a flow-rate of 1.2 ml/min. Retinol is monitored at 325 nm, alpha-tocopherol at 292 nm and beta-carotene at 450 nm. Serum is deproteinized with ethanol containing the internal standard (alpha-tocopherol acetate), then extracted with hexane. The evaporated organic layer is reconstituted with the mobile phase and injected. The choice of the eluent is discussed, as well as the choice of an internal standard and the need for an antioxidant during the extraction step. Sixteen different eluents are compared in terms of analysis time and selectivity. The linear concentration ranges (retinol 0.016-13.7 microM, alpha-tocopherol 0.18-91.8 microM, beta-carotene 0.05-5.75 microM), within-run coefficients of variation (retinol less than 7%; alpha-tocopherol less than 8%, beta-carotene less than 7%), between-run coefficients of variation (retinol less than 13%, alpha-tocopherol less than 9%, beta-carotene less than 8%) and recoveries (retinol greater than 95%, alpha-tocopherol greater than 91%, beta-carotene greater than 80%) are suitable for clinical investigations. Serum reference values were found to be 2.47 +/- 0.61 microM (retinol), 30.5 +/- 6.8 microM (alpha-tocopherol) and 0.91 +/- 0.55 microM (beta-carotene). A significant difference (p less than 0.001) between males and females was found for retinol. 相似文献
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巢湖、龙感湖水体中稀土元素的无机形态研究 总被引:7,自引:0,他引:7
运用MINTEQ化学平衡软件对巢湖、龙感湖中溶解态稀土的形态进行模拟。模拟结果表明,在巢湖和龙感湖中Ln(CO3)^2-,LnCO3^+是溶解态稀土的最主要的存在形式,当8pH〉7.19时,REE主要以LnCO3^+形式存在,当pH〉8时,REE主要以Ln(CO3)2^-形式存在,并且∑Ln(CO3)n^3-2n(n=1和2)形态的稀土基本上占溶解态稀土总含量的93%以上。Ln^3+在巢湖和龙感湖水体中平均丰度为5.03%,Ln^3+的丰度和pH值成反相关关系。LnPO4在湖水中平均丰度为1.61%,但这种形式的稀土在巢湖和龙感湖中非常重要。巢湖和龙感湖中LREE的LnPO4均处于过饱和状态,甚至巢湖西半湖区丰水期HREE的LnPO4的也都处于过饱和状态,PO4^3+对稀土的存在有很强的限制作用。InSO4,LnF^2+,LnOH^2+,LnCl^3+等形态的各元素平均丰度均小于1%,在富营养化的淡水中通常可以忽略不计。 相似文献
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Based on the adsorption of Fe(EDTA)- on a chitosan-coated glassy carbon electrode, a second-derivative square-wave voltammetry for the determination of the EDTA species in water samples was investigated. The measuring range of EDTA was from 6.0 x 10(-7) to 5.0 x 10(-5) mol/L with a correlation coefficient of 0.998 and a detection limit of 2.8 x 10(-7) mol/L. The relative standard deviation was less than 6.2% (n = 5) and the recovery was in the range of 98-105% for the determination of practical samples. The result was consistent with that from the HPLC method. 相似文献
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In this study, a rapid and sensitive high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) determination of primary As species in fish tissues and urine is reported. The separation was achieved on an Altima C18 column with a mobile phase containing citric acid and hexanesulfonic acid (pH 4.5). As(V), monomethylarsonic acid (MMA), As(III), dimethylarsinic acid (DMA) and arsenobetaine (AsB) were separated in less than 4 min with retention times of 83, 99, 130, 166 and 208 s, respectively. This separation of five species in less than 4 min should be attractive to those interested in As speciation. The quantification limits were 44, 56, 94, 64, 66 ng l(-1) and the relative standard deviations (R.S.D.) for day-to-day injections of As at 2 mug l(-1) were 2.0, 3.1, 2.4, 3.8 and 4.0%. The procedure was tested using two reference materials (DORM-2 dogfish muscle tissue, NIST SRM 2670 Freeze-dried Urine, normal level) and then applied to real-world samples. The results obtained demonstrate the suitability of the procedure for screening and quantification at physiological levels of primary As species in biological samples. 相似文献
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Stacchiola D Burkholder L Zheng T Weinert M Tysoe WT 《The journal of physical chemistry. B》2005,109(2):851-856
The chemisorptive enantioselectivity of propylene oxide is examined on Pd(111) surfaces templated by chiral 2-methylbutanoate and 2-aminobutanoate species. It has been found previously that chiral propylene oxide is chemisorbed enantiospecifically onto Pd(111) surfaces modified by either (R)- or (S)-2-butoxide. The enantiomeric excess (ee) varied with template coverage, reaching a maximum of approximately 31%. Templating the surface using 2-methylbutanoate, where the chiral center is identical to that in the 2-butoxide species, but is now anchored to the surface by a carboxylate rather than an alkoxide linkage, shows no enantiospecificity. The enantioselectivity is restored when the methyl group is replaced by an amine group, where a maximum ee value of approximately 27% is found. DFT calculations and infrared measurements suggest that the structures of the butyl group on the surface are similar for both 2-butoxide and 2-methylbutanoate species, implying that gross conformational changes are not responsible for differences in chemisorptive enantioselectivity. There is no clear correlation between the location of the chiral center and enantioselectivity, suggesting that differences in the template adsorption site are also not responsible for the lack of enantioselectivity. It is proposed that the 2-butyl group in 2-methylbutanoate species is less rigidly bonded to the surface than that in 2-butoxides, allowing the chiral center to rotate azimuthally. It is postulated that the role of the amino group in 2-aminobutanoate species is to anchor the chiral group to the surface to inhibit azimuthal rotation. 相似文献
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A laboratory-built automated instrument is reported for on-line, near real-time monitoring of nine haloacetic acids species (HAA9) in drinking water. The device uses anion-exchange chromatography to separate the HAA9 species, followed by post-column reaction with nicotinamide in basic solution with fluorescence detection. Method detection limits for HAA9 species ranged from 0.6 to 10.1 μg L−1, mean % recovery values ranged from 58 to 161%, and % relative standard deviation ranged from 3.5 to 32% while operating within a factor of 2.5-5 of the method detection limit. The bias between the proposed method and United States Environmental Protection Agency Method 552.3 was measured during two separate on-line studies and using grab samples collected from different distribution systems. In general, the two methods showed good agreement with biases for HAA9 of less than 10 μg L−1. 相似文献