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1.
A novel green method using flow injection chemiluminescence with controlled-reagent-release technology has been investigated for the rapid and sensitive monitoring of sub-nanogram amounts of chlorpyrifos. The analytical reagents involved in chemiluminescence (CL) reaction, luminol and periodate, were both immobilized on an anion-exchange column. The CL signals produced by the reaction between luminol and periodate, which were eluted from the column through water injection, were decreased in the presence of chlorpyrifos. The decrease of CL intensity was linear over the logarithm of concentration of chlorpyrifos ranging from 0.48 to 484.0 ng x mL(-1) (r(2) = 0.9969), and the limit of detection was 0.18 ng x mL(-1) (3sigma). At a flow rate of 2.0 mL x min(-1), the determination of chlorpyrifos, including sampling and washing, could be performed in 0.5 min with a relative standard deviation of less than <3.0%. The proposed method was applied successfully in an assay of remnant chlorpyrifos on fruits such as orange and shaddock with the recovery of 94.4-107.4%. The change of the concentration of chlorpyrifos in a water sample was also investigated, and the variation rate was 99.96% during 35 h in the open air.  相似文献   

2.
苏丹红Ⅰ直接竞争ELISA检测试剂盒的研制   总被引：2，自引：0，他引：2  
直接包被多克隆抗体建立了苏丹红ⅠELISA检测技术,研制苏丹红ⅠELISA检测试剂盒。结果表明,制备的多克隆抗体对苏丹红Ⅰ亲合力强、特异性高,试剂盒标准曲线呈典型的S型,符合4参数logit曲线拟合,线性范围为1.55～100μg/L,50%抑制率(IC50)为13.52μg/L,灵敏度(IC10)为1.95μg/L,平均批内与批间变异系数分别为7.6%与10.6%,与苏丹红Ⅱ、Ⅲ的交叉反应率分别为4.40%和1.70%,与苏丹红Ⅳ及其他违禁食品染色剂交叉反应率低于0.01%;干辣椒、辣椒粉、辣椒油与辣椒酱等4种样品的苏丹红平均添加回收率分别为88.1%、91.4%、78.2%和84.3%,最低检测限分别为1.82、1.71、2.19和2.12μg/kg;与HPLC检测方法具有较高的相符性,4种样品相关系数分别为0.95,0.94,0.86和0.87;该试剂盒在4℃下至少可保存180d,可用于辣椒及其制品中苏丹红Ⅰ的批量快速低成本筛查。  相似文献   

3.
A novel continuous-flow sensor based on chemiluminescence (CL) detection was developed for the determination of rutin in pharmaceutical preparations and human urine by controlled-reagent-release technology. The analytical reagents involved in the CL reaction, including luminol and hexacyanoferrate(III), were both immobilized on an anion-exchange column in a flow-injection system. The CL signal produced by the reaction between luminol and hexacyanoferrate(III), which were eluted from the column through sodium phosphate injection, was decreased in the presence of rutin. CL intensity was inhibited by rutin; the decrement of CL intensity was linear over the logarithm of the rutin concentration range of 1.0-400 ng x mL(-1), and the detection limit was 0.35 ng x mL(-1) (3 sigma). The whole process, including sampling and washing, could be completed in 1.5 min with a relative standard deviation of <3.5%. The flow sensor showed remarkable stability and could be easily reused >450 time; the sensor proposed was applied successfully to the determination of rutin in pharmaceutical preparations and human urine.  相似文献   

4.
A new single-hole hollow molecularly imprinted polymer (SHH-MIP) was prepared by multistep seed swelling polymerization using Sudan I as template molecule and successfully applied to selective solid-phase extraction (SPE) of Sudan dyes in chilli sauce samples. The polymers possessed high specific surface area obtained by nitrogen adsorption and good thermal stability without decomposition lower than 380 °C by thermogravimetry analysis. Much higher binding capacity was exhibited than with irregular solid MIP prepared by bulk polymerization, because most of the binding sites were located in the surface of the polymers, facilitating template removal and mass transfer. Accordingly, the SHH-MIP was employed as SPE adsorbent for chilli sauce analysis and offered high recoveries for Sudan I in the range of 87.5-103.4% with the precision of 1.94-5.33% at three spiked levels. The SHH-MIP with high selectivity and high stability was demonstrated to be potentially applicable for high selective preconcentration and determination of trace Sudan dyes in complicated samples.  相似文献   

5.
A new method based on partial filling micellar electrokinetic chromatography (MEKC) for the quantitative determination of Sudan dyes (I, II, III, and IV) in chilli sauces is presented. The separation is achieved filling 25% of the capillary with a MEKC buffer composed of 40 mM NH(4)HCO(3), 25 mM sodium dodecyl sulfate, and 32.5% (v/v) acetonitrile (ACN). The rest of the capillary is filled using a capillary zone electrophoresis (CZE) buffer composed of 40 mM NH(4)HCO(3) and 32.5% (v/v) ACN. Under optimized conditions, the azo dyes are baseline separated in less than 8 min with limits of detection ranging from 0.57 to 0.71 μg mL(-1) (S/N > 3). Using an internal standard, the repeatability of the quantitative determination is improved almost four times. The applicability of the method for rapid screening and determination of Sudan dyes is corroborated by analyzing spiked chilli sauce samples with recoveries from 85 to 99%. The reported conditions are demonstrated to be compatible with mass spectrometry detection.  相似文献   

6.
A highly selective imprinted polymer was synthesized by a surface molecular imprinting technique in combination with a sol-gel process. The imprinted polymer was evaluated by FT-IR and static and kinetic adsorption experiments. The results showed that the imprinted sorbent exhibited good recognition and selective ability, offered a faster kinetics for the adsorption and desorption of Sudan I than the non-imprinted sorbent, a saturated binding capacity (Qmax) that reached 33.47 mg g-1. The prepared sorbent was applied for the determination of trace Sudan I through on-line solid-phase coupled with high-performance liquid chromatography (SPE-HPLC). With a loading flow rate of 1.5 mL min-1 for sampling 50 mL, an enrichment factor of 1266 was achieved. The detection limit (S/N = 3) was 1.2 ng L-1, and the peak area precision (RSD) for five replicate detections of 0.01 microg L-1 Sudan I was 3.66%. The Sudan I in the chilli powder from the local market was determined at three levels (0.25, 0.5, and 1.0 ng g-1) with recoveries ranging from 80.31 to 94.02%.  相似文献   

7.
The antioxidant activities of three parts (peel, juice, and seed) and extracts of three pomegranate varieties in China were investigated by using a chemiluminescence (CL) method in vitro. The scavenging ability of pomegranate extracts (PEs) on superoxide anion, hydroxide radical, and hydrogen peroxide was determined by the pyrogallol-luminol system, the CuSO4-Phen-Vc-H2O2 system, and the luminol-H2O2 system, respectively. DNA damage preventing the effect of PE was determined by the CuSO4-Phen-Vc-H2O2-DNA CL system. The results showed that the peel extract of red pomegranate had the best effect on the scavenging ability of superoxide anion because its IC50 value (4.01 +/- 0.09 microg/mL) was the lowest in all PEs. The seed extract of white pomegranate could scavenge hydroxide radical most effectively of the nine extracts (the IC50 value was 1.69 +/- 0.03 microg/mL). The peel extract of white pomegranate had the best scavenging ability on hydrogen peroxide, which had the lowest IC50 value (0.032 +/- 0.003 microg/mL) in the nine extracts. The seed extract of white pomegranate (the IC50 value was 3.67 +/- 0.03 microg/mL) was the most powerful on the DNA damage-preventing effect in all of the PEs. Also, the statistical analysis indicated that there were significant differences (at P < 0.05) among the extracts of the different varieties and parts in each system.  相似文献   

8.
A liquid chromatography (LC) method with luminescence detection for the determination of eight quinolone antibiotics is reported. The system encompasses three consecutive steps: (a) chromatographic separation using reverse-phase mode (RP-LC), (b) postcolumn derivatization reaction, and (c) luminescence detection by monitoring fluorescence (FL) and time-resolved (TR) signals. The derivatization step is based on the reaction between quinolones and terbium(III) to form luminescent chelates, which were determined at lambda(ex) 340 and lambda(em) 545 nm (FL mode) or at lambda(ex) 281 and lambda(em) 545 nm (TR mode). Dynamic ranges of the calibration graphs, obtained with standard solutions of analytes and FL and TR modes, respectively, were 190-3500 and 316-2000 ng mL-1 for marbofloxacin, 8-3500 and 8.1-1500 ng mL-1 for ciprofloxacin, 6.2-3500 and 13-1500 ng mL-1 for danofloxacin, 7.4-3500 and 8.4-1500 ng mL-1 for enrofloxacin, 14-3500 and 20-2000 ng mL-1 for sarafloxacin, 12.5-3500 and 13.9-1200 ng mL-1 for difloxacin, 7.6-3500 and 13-3000 ng mL-1 for oxolinic acid, and 9-2000 and 130-3000 ng mL-1 for flumequine. Limit of detection values obtained using FL and TR modes, respectively, were 60 and 95 ng mL-1 for marbofloxacin, 2 and 2.4 ng mL-1 for ciprofloxacin, 1.9 and 3.9 ng mL-1 for danofloxacin, 2.2 and 2.5 ng mL-1 for enrofloxacin, 3.8 and 7 ng mL-1 for sarafloxacin, 4 and 4.2 ng mL-1 for difloxacin, 2.3 and 4 ng mL-1 for oxolinic acid, and 2.7 and 40 ng mL-1 for flumequine. The precision was established at two concentration levels of each analyte and expressed as the percentage of relative standard deviation with values ranging between 1.9 and 7.8%. The validation procedure for the analysis of samples was carried out using European Community recommendations, and the decision limit and detection capability were calculated for bovine whole milk. The method was applied to whole, semiskimmed, and skimmed milk samples spiked with the target analytes, and the recoveries ranged between 93.3 and 106.0%.  相似文献   

9.
A novel chemiluminescence method for the determination of antu has been developed based on the reaction between potassium permanganate in acid medium with this rat-poison in the presence of formaldehyde as an emission enhancer. The main feature of the system used is that the recording of the whole chemiluminescence intensity-vs-time profiles can be obtained, using the stopped-flow technique in a continuous-flow system. This enables the use of three quantitative parameters adjustable via software settings, one of them a typically kinetic parameter, such as rate of the light-decay reaction, and the others conventional parameters, such as maximum emission intensity and total emission area, which are proportional to the analyte concentration. The optimum chemical conditions for the chemiluminescence emission were investigated. The effect of common emission enhancers, such as formic acid, formaldehyde, glutaraldehyde, acetaldehyde, quinine, fluorescein, rhodamine B, and rhodamine 6G, was studied. The parameters selected were sulfuric acid 4.0 mol L(-)(1), permanganate 0.1 mmol L(-)(1), and formaldehyde 1.0 mol L(-)(1). The calibration graphs obtained with each one of the measurement parameters were linear for the concentration range from 0.05 to 3.00 microg mL(-)(1). The detection limits ranged from 0.005 to 0.010 microg mL(-)(1), and RSD values (n = 10) of 0.99-1.79% at a 0.30 microg mL(-)(1) concentration level and 1.71-2.22% at a 1.0 microg mL(-)(1) concentration level were obtained. The present chemiluminescence procedures were applied to the determination of antu in different kinds of samples, such as river water, wheat, barley, and oat grain samples. Recovery values not significantly different from the spiked amount were found for these determinations.  相似文献   

10.
Anionic soybean peroxidase Glycine max (SbP) is shown to efficiently catalyze luminol oxidation by hydrogen peroxide. Contrary to horseradish peroxidase, the presence of p-iodophenol in the reaction medium affects slightly the efficiency of SbP catalysis. A maximal intensity of chemiluminescence, produced through this enzymatic reaction, was detected at pH 8.4-8.6. Contrary to anionic palm tree peroxidase, in the presence of SbP, chemiluminescence intensity increases with the reaction buffer concentration. The detection limit of SbP in the reaction of luminol oxidation is 0.3 x 10(-12) M. Therefore, high sensitivity in combination with the long-term chemiluminescent signal is indicative of good prospects for application of this enzyme in enzyme immunoassay with chemiluminescent detection.  相似文献   

11.
为了快速的检测癌胚抗原(CEA),将胶体金与适配体室温孵育后加入CEA以及氯化钠溶液,随着CEA浓度的增加,分析胶体金溶液颜色的变化情况。结果表明,试验中含有2种不同核酸适配体(18个碱基和19个碱基)的胶体金溶液,其颜色都是随着CEA浓度增加均呈梯度变化,颜色梯度为从酒红色到深蓝色。实际样品的检测结果也呈现出良好的颜色梯度变化,CEA检测限为2 ng·mL~(-1),检测范围为0~200 ng·mL~(-1),且检测方法特异性良好。本研究结果为疾病的前期诊断提供了简便快速廉价的检测方案。  相似文献   

12.
我国大蒜废弃物资源丰富,为引导其合理化、资源化利用,测定了大蒜提取物对大豆尖孢镰刀菌（Fusarium oxysporum fsp.tracheiphilum）、油菜菌核病菌（Sclerotinia sclerotiorum（Lib.）d eBary）、大豆细菌性斑点病菌（Pseudomonas.s yringae pv.glycinea）和水稻白叶枯病菌（Xanthomonas oryzae pv.oryzae〔Ishiyama〕Dye,Xoo）4种植物病原菌的抑制作用,并通过大蒜提取物、大蒜渣、大蒜肥对土壤中大豆尖孢镰刀菌的抑制试验,测定了其在土壤中对土传病原菌的抑制效果。结果表明,高浓度的大蒜提取物对这4种植物病原菌有抑制作用,随着提取物浓度的升高,抑菌效果也更为明显。质量浓度为500mg.mL-1时对大豆尖孢镰刀菌、大豆细菌性斑点病菌和水稻白叶枯病菌的抑菌效果最好。培养基中提取物浓度达100mg.mL-1时对两种真菌的抑制达100%。同时,含大蒜提取物0.05mL.g-1、大蒜渣5%或大蒜肥25%的土壤能抑制土传病原菌大豆尖孢镰刀菌在土壤中的定殖。  相似文献   

13.
A method for the determination of DNA based on the fluorescence intensity of the gatifloxacin-europium(III) (GFLX-Eu(3+)) complex that could be enhanced by DNA was developed. The GFLX-Eu(3+) complex showed an up to 6-fold enhancement of luminescence intensity after adding DNA. Under the optimized experimental conditions, the system exhibited a linear relationship between the enhanced fluorescence intensity and the concentration of calf thymus DNA (ctDNA) over the range from 1.0 × 10(-8) to 1.5 × 10(-6) g mL(-1), with a correlation coefficient (R) of 0.997, and the detection limit (3σ) of the method was determined as 6.0 × 10(-9) g mL(-1). The mechanism of the fluorescence enhancement effect was also discussed.  相似文献   

14.
Bovine somatotropin (bST) and insulin-like growth factor-1 (IGF-1) are peptide hormones that are involved in the regulation of milk production in dairy cows. Because these hormones are present at extremely low concentration in fresh and processed bovine milk, a highly sensitive and specific electrochemiluminescent immunoassay (ECLIA) has been developed to better estimate the concentration of these hormones in milk. The assay employs an imager, a capture antibody bound to a carbon electrode, and a detection antibody coupled to a ruthenium label. In the presence of tripropylamine and an electric pulse, ruthenium generates light proportional to the amount of antigen bound, and the light is captured as signal by a charge-coupled device (CCD) camera. Using bovine milk as the starting matrix, 99.69% of bST and 104.79% of IGF-1 were recoverable. The limit of detection (LOD) was <5 pg/mL for bST and <1 pg/mL for IGF-1. The limit of quantification (LOQ) was <14 pg/mL for bST in milk and <2 pg/mL of IGF-1. The assay is highly specific and shows <0.2% cross-reactivity with other peptide hormones found in bovine milk such as insulin and IGF-2. These data indicate this new, ECLIA is highly sensitive and specific for estimating the concentration of bST or IGF-1 in milk.  相似文献   

15.
In this paper, a novel and sensitive method based on Rayleigh light scattering technique (RLS) was proposed for the determination of sulfate using a conventional spectrofluorometer. Sulfate was transformed to BaSO4 particles, which displayed intense light scattering in aqueous solutions. The effects of factors such as wavelength, acidity, stabilizers and interferents were studied in detail. The RLS intensity of the BaSO4 suspension was obtained in 0.1 mol L(-1) of [H+] and the addition of 2 mL of cationic polyacrylamide (CPAM) with 7.05 x 10(-3) mmol mL(-1) charged cations and 1.0 mL of BaCl2.2H2O (5.0%) at 510 nm. In the range of 8-400 microg mL(-1), RLS intensity was linear to the concentration of BaSO4, and the detection limit was 0.3 microg mL(-1). To determine the feasibility of the proposed method, some samples of water, drinks, and vegetables digests were analyzed, and the results were in agreement with the standard turbidimetric method. Good recovery results were also obtained in the range of 94-105%. Although this method was limited in stability, it was characterized with simplicity, sensitivity, reliability, and little interference.  相似文献   

16.
1,5-bis(p-Hydroxybenzaldene)thiocarbohydrazone (BHBTZ) had been synthesized and used as a new kind of substrate for horseradish peroxidase (HRP). The experiment results showed that ascorbic acid (AsA) had strongly inhibiting effect on the BHBTZ-H(2)O(2)-HRP reaction system, so AsA had been spectrophotomericly determined as the inhibitor by enzymatic inhibition method. Under experimental conditions, the linear relationship between DeltaA(386) and AsA concentration was in the range of 0.82-18.0 microg ml(-1) with a detection limit of 0.245 microg ml(-1). The effect of interferences on AsA determination was investigated. The proposed method was successfully applied to the determination of AsA in tea drink.  相似文献   

17.
为探明光照对水稻根、叶界面氮氧化物排放的调控机制,用密闭箱法,探讨了光照对开花结实期水稻叶际及根际氮氧化物排放的影响。结果表明,相同氮源(NH4NO3-N,N质量浓度90 mg/L),日间光照为6 000、8 000 lx条件下,同期水稻叶际N2O和NO排放速率分别为27.08、29.15μg/(盆·h)和2.25、0.94μg/(盆·h),分别占N2O和NO总排放的57.38%、54.19%和76.79%、51.93%;光强(1 600 lx)一致条件下,同期用发光二极管控制的黄、绿、白、红、蓝光处理水稻叶际N2O排放速率分别为2.16、13.40、1.07、3.82和7.08μg/(盆·h),红、蓝光在抑制水稻叶际N2O及根际NO排放的同时,有效提高了水稻根际N2O排放速率;相同条件下,红、白光能促进叶际NO排放,蓝光明显抑制了水稻根、叶界面NO排放,但水稻根、叶界面均无明显的NO2净排放作用(P0.05);0~8 000 lx范围内,水稻根、叶界面N2O及根际NO排放随光强增加而增加,但高光强(8 000 lx)处理有降低叶际NO排放作用(P0.05)。从试验结果看,水稻根、叶界面排放的90%以上的氮氧化物是N2O,且叶际N2O排放受根际N2O控制。研究表明适度增加红、蓝光比例并依据供氮水平同步调节光强,可有效抑制水稻根、叶界面氮氧化物排放。研究结果为水稻开花结实期根、叶界面气态氮氧化物减排的光控技术提供了重要依据和参考。  相似文献   

18.
An on-line HPLC-DPPH screening method for phenolic antioxidants in apple methanol/water (80:20, v/v) extracts was applied. The determination of antioxidants was based on a decrease in absorbance at 515 nm after postcolumn reaction of HPLC-separated antioxidants with the 2,2'-diphenyl-1-picrylhydrazyl radicals (DPPH*). Each of the antioxidants separated by the HPLC column was observed as a negative peak corresponding to its antioxidative activity. The on-line method was applied for quantitative analysis of the antioxidants. A linear dependence of negative peak area on concentration of the reference antioxidants was observed. For validation of the on-line method the limit of detection, LOD (microg/mL), and the limit of quantification, LOQ (microg/mL), of the phenolic compounds were determined. Comparison of the UV and DPPH radical quenching chromatograms with authentic compounds identified catechin, chlorogenic acid, caffeic acid, epicatechin, and phloridzin in the apple cultivars (Lobo, Golden Delicious, and Boskoop), and the distribution of total antioxidant activity was calculated.  相似文献   

19.
徐淮平原农田防护林带杨树树干液流研究   总被引：12，自引：1，他引：12       下载免费PDF全文
 为了揭示农田防护林带对附近农作物产生的胁地机制,为农田防护林带的树种配置和制定克服胁地的措施提供理论依据。用热脉冲技术,采用ICT2000TE树干液流测定系统,研究8年生NL80105杨和11年生I69杨生长盛期树干液流的特点及其与环境因子的关系。结果表明:1)NL80105杨和I69杨的单位面积液流通量,分别为0.244L/(cm2 ·d)和0.172L/(cm2 ·d),I69杨的蒸腾耗水强度较NL80105杨的大;2)NL80105杨和I69杨液流的日进程,均呈低—高—低的变化趋势;3)NL80105杨和I69杨,均存在夜间明显的树干液流上升现象。  相似文献   

20.
为了降低大豆酱油的含盐量,该文利用电渗析技术对大豆酱油进行脱盐处理,通过单因素试验探讨了电压、流速、pH值对电渗析脱盐效果的影响,确定了较佳电渗析工艺。结果表明在电压为9 V,流速为2.4 cm/s,pH值为4.2,电渗析50 min时脱盐效果较好,氨基酸态氮损失较小,氨基酸态氮损失19.4%,脱盐率达到81.6%。利用氨基酸自动分析仪和气相色谱-质谱联用仪（gas chromatography-mass spectrometry）分析了电渗析前后游离氨基酸及挥发性风味物质的变化规律,结果表明电渗析过程中氨基酸及风味物质均有损失。几种苦味氨基酸如组氨酸、精氨酸、赖氨酸损失较大,分别损失了23.79%、26.39%和28.5%;电渗析过程中,酱油风味物质中醇类、酚类损失较大,尤其是4-乙基愈创木酚损失最多,但因其气味阈值较低,因此对酱油风味影响较小。研究结果为减盐酱油系列产品的生产提供了参考和依据。  相似文献   

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