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1.
综述了目前国内外微囊藻毒素检测方面的各种研究方法及成果,对高效液相色谱(HPLC)、液相色谱串联质谱(LC–MS)、气相色谱串联质谱(LC–MS)、毛细管电泳(CE)、薄层色谱(TLC)、生物法和生物化学法等检测方法存在的优缺点进行了评述,并展望了该研究领域的未来发展趋势。  相似文献   

2.
高效液相色谱法检测水体中微囊藻毒素   总被引:6,自引:2,他引:6  
建立了高效液相色谱检测水体中微囊藻毒素(Microcystins,MCs)的方法.选择XAD-2树脂为富集树脂,采用四氯化碳-10%乙醇-10%丙酮连续淋洗,获得较好的杂质去除效果,采用90%甲醇可以将树脂柱上的MCs完全洗脱.HPLC采用V(0.1% TFA):V(甲醇)=42: 58混合溶液为流动相进行等度洗脱,MC-RR和 MC-LR取得较好分离效果,回收率均达到90%以上.水样富集2000倍后,方法的检出限为0.05 μg/L.本方法操作简便、灵敏度高、检测速度快.  相似文献   

3.
免疫亲和层析-液质联用法检测蓝藻中的微囊藻毒素   总被引:2,自引:1,他引:2  
应用自制的微囊藻毒素(microcystin,MC)免疫亲和层析柱为净化工具,建立了固相萃取柱富集、免疫亲和层析柱净化、液质联用法检测蓝藻样品中MC的方法.结果显示:只用固相萃取柱富集,会残留大量杂质,干扰MC(尤其是MC-LR)的测定结果.而用免疫亲和层析柱净化能有效去除藻样中的杂质,排除干扰,通过液质联用法定量,能准确测定藻样中的微囊藻毒素-RR(MC-RR)和-微囊藻毒素-LR(MC-LR).方法的检出限为2.5 μg/L; 线性范围为5~500 μg/L; MC-RR和MC-LR平均回收率高于84%; 相对标准偏差低于5%.  相似文献   

4.
在玻碳电极表面修饰碳纳米管,并用多电位阶跃法在碳纳米管表面沉积纳米金制得碳纳米管/纳米金复合膜。通过纳米金和微囊藻毒素-(亮氨酸-精氨酸)抗体之间的吸附作用,将抗微囊藻单克隆抗体固定于电极表面,以牛血清白蛋白封闭非特异性吸附位点,研制了检测微囊藻毒素的电化学免疫传感器。利用微囊藻毒素与其抗体之间的特异性识别作用构建"三明治"夹心结构的免疫分析模式,以辣根过氧化物酶标记抗体为二抗,利用微分脉冲伏安法实现了对微囊藻毒素的检测。在优化条件下,此传感器的响应电流与微囊藻毒素浓度在0.50~12.0μg/L范围内呈良好的线性关系,检出限为0.30μg/L(S/N=3)。对实际水样进行了微囊藻毒素的加标回收实验,回收率在93.0%~108.5%之间,相对标准偏差为3.8%~5.0%。  相似文献   

5.
用CNBr-activated Sepharose4B和微囊藻毒素-LR的单克隆抗体制备了免疫亲和层析柱,测得抗体偶联率在75.7%~94.1%之间。制得的免疫亲和层析柱最大柱容量在76~95ng之间,柱空白为0,回收率在90.8%~105.1%之间。柱子再生重复使用6次后,回收率不低于75%。建立了免疫亲和层析柱-高效液相色谱测定水样中的微囊藻毒素-LR的方法。该法检出限为5ng/L;线性定量范围为10~500ng/L。实验结果显示,免疫亲和层析柱特异性好,一次净化能除去绝大部分干扰物,净化效果明显优于现有的固相萃取柱。  相似文献   

6.
利用石墨烯纳米片层(GS)偶联牛血清白蛋白(BSA)标记的微囊藻毒素(MCLR)(BSA-MCLR)构建了纳米金(Au NPs)为信号探针的电流型免疫传感器。分别用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和紫外-可见吸收光谱对合成纳米材料进行表征;用循环伏安法研究修饰电极表面的电化学特性。通过待测MCLR与固定的BSA-MCLR竞争结合抗体(anti-MCLR),之后恒电位将Au NPs氧化为Au Cl-4,再利用差分脉冲伏安法(DPV)进行阴极电位扫描,还原Au Cl-4为Au,以产生的峰电流值为检测信号,测定MCLR浓度。最佳实验条件下,用免疫传感器测定MCLR的线性范围为0.1~50μg/L,检出限为0.05μg/L。对传感器的重现性、稳定性和选择性进行了考察。相较于酶标探针,以Au NPs为信号探针标记抗体,可使检测过程更经济便捷,稳定性更强,检测效果良好。  相似文献   

7.
Fan S  Zhao R  Li B  Liu W  Wu G 《色谱》2012,30(5):434-439
微囊藻毒素是蓝藻暴发中出现频率最高、产生量最大和造成危害最严重的藻毒素,具有多器官毒性、遗传毒性和致癌性。水产品中微囊藻毒素的残留会对人体产生危害,并对我国公众健康构成巨大威胁。因此,水产品中微囊藻毒素的检测和控制变得非常重要,迫切需要建立一种简便、快速、灵敏度较高的检测方法,以对水产品中的微囊藻毒素进行监控。为加强水产品中微囊藻毒素的痕量分析技术研究,对水产品中残留的微囊藻毒素开展监测,综述了国内外有关水产品中微囊藻毒素污染检测的提取、净化及分析技术进展。  相似文献   

8.
微囊藻毒素是常见的蓝藻毒素,具有很强的肝脏神经系统和肾脏毒性. 由于水的富营养化,蓝藻会爆发产生大量的微囊藻毒素,进而对水生生物和食用它们的人类构成巨大威胁. 随着浓缩、富集、分离方法和仪器技术的进步,定量分析微囊藻毒素的方法也在不断进步,且应用越来越广泛. 综述了水、沉积物和生物中微囊藻毒素的富集和检测方法,结果显示:目前常见的采样方法是主动采样法,开发简便可靠和实用的被动采样方法是急需的研究方向之一. 衍生化方法可以降低基质效应,有利于使用不同的检测方法和试验观察,因此开发一种高效、灵敏的衍生化方法检测微囊藻毒素将是重要的研究方向之一.  相似文献   

9.
经稀酸提取和固相萃取柱富集微囊藻毒素(MC)后,采用反相高效液相色谱测定蓝藻水华中的MC-RR-、YR-、LR。考察了在300SBZorbax C18柱(250×4.6 mm i.d.,5μm)上流动相中乙腈含量、三氟乙酸浓度以及温度对分离的影响。在等度及梯度洗脱条件下,三种毒素均被完全分离,梯度洗脱时峰形更好,检测灵敏度较高。方法对蓝藻干粉中MC的检出限为20 ng/g,线性范围为0.06~6μg/g,回收率91.7%~102.1%。此方法灵敏度高,实用性强,可作为水质藻毒素风险评价和监测蓝藻脱毒效能较可靠的分析方法。  相似文献   

10.
本研究在玻碳电极(GCE)表面电沉积金纳米粒子(Au NPs),通过化学吸附将微囊藻毒素-(亮氨酸-精氨酸)(MC-LR)的单克隆抗体(anti-MC-LR)固定在电沉积了Au NPs的玻碳电极表面,以牛血清白蛋白(BSA)封闭非特异性吸附位点,制得免疫电极anti-MC-LR/Au NPs/GCE。采用微乳化法制备了掺杂三(2,2'-联二吡啶)钌(Ⅱ)配合物离子(Ru(bpy)2+3)的二氧化硅纳米粒子(Ru@SiO2),利用透射电镜和扫描电镜对所制备的纳米粒子进行表征。3-氨基丙基三乙氧基硅烷(APTS)进一步与Ru@SiO2反应,制得氨基功能化的Ru@SiO2,通过1-(3-二甲氨基丙基)-3-乙基碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)活化辣根过氧化物酶标记的MC-LR(HRP-MC-LR),并使其与氨基功能化的Ru@SiO2偶联,制得MC-LR-Ru@SiO2。采用直接竞争模式,在标记物MC-LR-Ru@SiO2存在下,以三丙胺作为共反应物,利用电化学发光法(ECL)测定溶液中的微囊藻毒素,免疫反应完成后,电化学发光强度(I)随着MC-LR浓度的增大而减小,且在0.100~100μg/L范围内,电化学发光强度差值(ΔI)与游离的MC-LR浓度的对数呈良好线性关系,检出限为0.007μg/L。对实际水样进行了加标回收实验,回收率为95.5%~105%。  相似文献   

11.
Nanofibers featuring functional nanoassemblies show great promise as enabling constituents for a diverse range of applications in areas such as tissue engineering, sensing, optoelectronics, and nanophotonics due to their controlled organization and architecture. An infusion gyration method is reported that enables the production of nanofibers with inherent biological functions by simply adjusting the flow rate of a polymer solution. Sufficient polymer chain entanglement is obtained at Berry number > 1.6 to make bead‐free fibers integrated with gold nanoparticles and proteins, in the diameter range of 117–216 nm. Integration of gold nanoparticles into the nanofiber assembly is followed using a gold‐binding peptide tag genetically conjugated to red fluorescence protein (DsRed). Fluorescence microscopy analysis corroborated with Fourier transform infrared spectroscopy (FTIR) data confirms the integration of the engineered red fluorescence protein with the nanofibers. The gold nanoparticle decorated nanofibers having red fluorescence protein as an integral part keep their biological functionality including copper‐induced fluorescence quenching of the DsRed protein due to its selective Cu+2 binding. Thus, coupling the infusion gyration method in this way offers a simple nanoscale assembly approach to integrate a diverse repertoire of protein functionalities into nanofibers to generate biohybrid materials for imaging, sensing, and biomaterial applications.

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12.
Aligned poly(l ‐lactide)/poly(methyl methacrylate) binary blend fibers and mats loaded with a chimeric green fluorescence protein having a bioactive peptide with hydroxyapatite binding and mineralization property are prepared by pressurized gyration. The effect of processing parameters on the product morphologies, and the shape memory properties of these samples are investigated. Integration of hydroxyapatite nanoparticles into the fiber assembly is self‐directed using the hydroxyapatite‐binding property of the peptide genetically engineered to green fluorescence protein. Fluorescence microscopy analysis corroborated with Fourier transform infrared spectroscopy (FTIR) data confirms the integration of the chimeric protein with the fibers. An enzyme based remineralization assay is conducted to study the effects of peptide‐mediated mineralization within the fiber mats. Raman and FTIR spectral changes observed following the peptide‐mediated mineralization provides an initial step toward a soft‐hard material transition. These results show that programmable shape memory properties can be obtained by incorporating genetically engineered bioactive peptide domains into polymer fibers.

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13.
The influence of solute hydrophobicity and charge on partitioning and diffusion in physically crosslinked networks of a genetically engineered SELP polymer was investigated. A series of fluorescent dyes were used to assess the impact of solute charge and hydrophobicity on release behavior. The mechanism of solute release from the SELP hydrogel appeared to vary as a function of dye hydrophobicity. The extent of FITC attachment to amine‐terminated G4 dendrimers influenced SELP hydrogel partitioning more than dendrimer diffusion properties. Results suggest the possibility of controlling solute release from SELP hydrogels by modifying the hydrophobicity and surface charge of drugs and drug/polymer conjugates as well as the possibility of “designing‐in” solute‐specific interactions.

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14.
建立饮用水中微囊藻毒素(MC–RR,MC–LR)的超高效液相色谱–串联质谱检测方法。样品经PVDF针式过滤头过滤后直接进样,采用喷雾正离子源(ESI~+)和多重反应监测模式(MRM)测定。MC–RR的质量浓度在0.02~10.00μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.998 9,检出限为0.096μg/L,测定结果的相对标准偏差为6.6%~9.1%(n=7),加标回收率为99.0%~103.0%。MC–LR的质量浓度在0.1~20μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.999 2,检出限为0.188μg/L,测定结果的相对标准偏差为4.3%~10.0%(n=7),加标回收率为93.0%~114.0%。该方法灵敏度高、重现性好,可用于饮用水中微囊藻毒素的检测。  相似文献   

15.
Haptens of dichlorvos and paraoxon were conjugated to the carrier proteins of bovine serum albumin. The obtained conjugates were characterized by infrared and ultraviolet–visible spectroscopy. The binding ratios of dichlorvos and paraoxon-to-carrier proteins were also evaluated. The number of hapten molecules per protein molecule of dichlorvos–cationized bovine serum albumin conjugate was higher than for paraoxon–bovine serum albumin conjugate. The sheep polyclonal antibodies were produced against the dichlorvos and paraoxon. New multipolyclonal antibodies were obtained and characterized following the immunization of a 1:1 mixture of the immunogens for the simultaneous determination of dichlorvos and paraoxon by the immunoassay. An indirect enzyme-linked immunosorbent assay was used to characterize the reactivity of the antibodies to hapten conjugates. The multiantibodies showed lower affinities than the separate antibodies, but their affinities were sufficient for an immunoassay for the simultaneous determination of the analytes. The detection limit and linear range for the determination of dichlorvos and paraoxon alone and together were determined. The recovery was characterized to determine dichlorvos and paraoxon fortified in model solutions and milk. These results demonstrate the potential of this immunoassay for the quantitative screening of dichlorvos and paraoxon.  相似文献   

16.
Analytical limitations have constrained the determination of nanopollution character from real-world sources such as nano-enabled products (NEPs), thus hindering the development of environmental safety guidelines for engineered nanomaterials (ENMs). This study examined the properties of ENMs in 18 commercial products: sunscreens, personal care products, clothing, and paints—products exhibiting medium to a high potential for environmental nanopollution. It was found that 17 of the products contained ENMs; 9, 3, 3, and 2 were incorporated with nTiO2, nAg, binaries of nZnO + nTiO2, and nTiO2 + nAg, respectively. Commonly, the nTiO2 were elongated or angular, whereas nAg and nZnO were near-spherical and angular in morphology, respectively. The size ranges (width × length) were 7–48 × 14–200, 34–35 × 37–38, and 18–28 nm for nTiO2, nZnO, and nAg respectively. All ENMs were negatively charged. The total concentration of Ti, Zn, and Ag in the NEPs were 2.3 × 10−4–4.3%, 3.4–4.3%, and 1.0 × 10−4–11.3 × 10−3%, respectively. The study determined some key ENM characteristics required for environmental risk assessment; however, challenges persist regarding the accurate determination of the concentration in NEPs. Overall, the study confirmed NEPs as actual sources of nanopollution; hence, scenario-specific efforts are recommended to quantify their loads into water resources.  相似文献   

17.
《Analytical letters》2012,45(13):2563-2609
ABSTRACT

There are many compounds that require analysis ranging from pesticide levels in corn to disease markers in human patients. There are copious challenges to be met when measuring analytes such as the matrix in which they are to be determined, the amounts present, the cost and the rapidity of the result required. Enzyme immunoassays, immunoaffinity chromatography, immunomagnetic polymerase chain reaction, flow cytometry and immunobiological biosensors have all characteristics that can enhance analytical techniques. Antibody-based methods have found applications in a large number of diverse areas such as food and water analysis, clinical diagnosis and therapeutics The structure and modes of production of antibodies and antibody-based derivatives is described and their applications in analysis critically examined.  相似文献   

18.
介绍了人工模拟抗体的概念和制备方法,综述了人工模拟抗体在三嗪类农药、有机磷农药、苯氧羧酸类农药及其他农药残留检测中的应用,并对人工模拟抗体的发展作了展望(引用文献31篇)。  相似文献   

19.
洗涤用品是日常使用的产品,其质量安全受到广大消费者的关注。洗涤用品中可能存在的化学风险物质,将对消费者的健康安全产生负面影响。为了减少和避免洗涤用品质量安全问题,研究人员采用多种分析测试技术,开发、建立了洗涤用品中化学风险物质的检测方法。该文综述了近年来洗涤用品质量安全检测技术的研究进展,以期为相关领域的科技人员提供理论支持和技术参考。  相似文献   

20.
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