Research progress of rapid detection of typical environmental pollutants based on chromatographic technologiesEI北大核心CSCD

对复杂环境介质中的典型污染物进行快速、精准甚至远程连续自动的检测,是控制环境污染、确保环境和生态安全的重要前提。近年来,基于色谱技术的典型环境污染物快速检测方法发展迅猛,主要包括样品快速制备和目标物快速检测两方面。辅助萃取、快速液相萃取、QuEChERS等样品前处理方法具有萃取效率高、溶剂消耗少、操作简便快速等优点。快速检测技术可在几秒到半小时内提供检测结果,主要包括实验室和现场检测。本文综述了2019年以来基于色谱技术的典型环境污染物快速检测研究新进展。介绍了萃取技术和基于试验设计的样品快速制备,实验室快速检测、便携仪器现场检测及遥感技术远程检测,提出了色谱技术快速检测环境污染物的挑战和展望。     

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7种食品安全快检方法认定范围公布为规范餐饮服务食品安全监督执法中快速检测方法的使用,确保快速检测工作的科学与公正,根据《关于印发餐饮服务食品安全快速检测方法认定管理办法的通知》(国食药监食〔2011〕294号)规定,经研究,现将第一批餐饮服务食品安全快速检测方法认定范围公告如下:     

超高效液相色谱-四极杆飞行时间质谱法非靶向快速筛查进口粮谷中未知的农药残留

利用快速提取农药(fast pesticide extraction,FaPEx)方法前处理样品,并结合超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF)技术建立了非靶向快速筛查进口粮谷中未知的多种农药残留方法。采用1%(v/v)醋酸乙腈溶液提取粮谷中未知的农药残留,FaPEx固相萃取柱净化、浓缩,UPLC-Q-TOF检测。利用目标化合物特征离子的精确质量数、同位素匹配、二级碎片信息和保留时间进行数据库匹配,筛查可疑未知农药。结果表明,该方法无需对照标准品即可快速筛查进口粮谷中的农药残留,能够应用于进口粮谷样品的实际筛查。该方法快速、准确、分析通量高,可以为进口粮谷中农药残留的快速筛查和质量控制提供重要的方法依据。     

7种食品安全快检方法认定范围公布

为规范餐饮服务食品安全监督执法中快速检测方法的使用,确保快速检测工作的科学与公正,根据《关于印发餐饮服务食品安全快速检测方法认定管理办法的通知》（国食药监食[2011]294号）规定,经研究,现将第一批餐饮服务食品安全陕速检测方法认定范围公告如下：     

蓖麻毒素的间接酶联免疫快速检测

建立了间接酶联免疫法快速检测蓖麻毒素的方法。方法的线性范围在0.08~1.25 mg/L之间,相关系数r=0.992 3,检出限为0.02 mg/L。将该法用于检测实际水样、土壤、奶粉和血液蓖麻毒素加标样品,回收率在60%~98%范围。该方法简单、快速、假阳性率低,非常适合蓖麻毒素的快速筛选、定性和半定量分析。     

能量色散-X射线荧光光谱测定中草药痕量镉、铅、铜

为寻求一种能够直接对中草药中重金属进行快速检测的方法,采用压片法对样品进行前处理,建立了能量色散-X射线荧光光谱法快速检测中草药中痕量重金属镉、铅、铜元素的方法。在20 min即可完成检测,镉、铅、铜检出限分别为0.072、0.207、0.340 mg/kg,测试结果表明与原子吸收和ICP-MS相比,本方法数据稳定性和准确度良好,具有快速、准确、简单的优点,能够满足药典中对重金属元素的限量要求,适用于现场快速检测与质量控制检测。     

食源性致病菌快速检测方法研究进展

食源性致病菌污染是导致食品安全问题的重要因素,食源性致病菌的检测已成为近年来研究的热点。以免疫分析、分子生物学、生物传感器、代谢组学、核酸适配体等技术为基础的快速检测方法发展迅速,已成为检测食源性致病菌的主要方法。该文结合近年来各种快速检测方法的相关研究进展,介绍了以上述技术为基础的快速检测食源性致病菌的方法,并讨论了现有方法存在的问题和未来的发展方向,以期为食源性致病菌的防控和保障消费者身心健康提供借鉴。     

快速血糖仪应用于急诊检验血糖的价值分析

目的探讨分析快速血糖仪在急诊检验血糖中的应用价值。方法随机选取2014年7月—2015年7月间,于佛山市第一人民医院急诊科行快速血糖仪和常规生化仪检验血糖的90例患者参与此次研究。根据患者的临床资料,对两种检查方法的效果进行比较分析,并对快速血糖仪应用于急诊检验血糖的价值进行回顾性分析。结果经观察比较,快速血糖仪检查的90例患者的平均血糖值为(8.12±2.13)mmol/L,常规生化仪检验的90例患者的平均血糖值为(7.56±2.63)mmol/L,两种检查方法的结果比较无明显差异,无统计学意义(P0.05);快速血糖仪检查的90例患者的平均检测用时为(4.12±1.13)min,常规生化仪检验的90例患者的平均检测用时为(34.12±10.13)min,快速血糖仪检查方法明显较常规生化仪检验方法用时短,有明显差异,有统计学意义(P0.05)。结论快速血糖仪应用于急诊检验血糖的价值是确切可靠的。不仅较常规生化仪检验血糖用时更短,而且两种检查方法的检测结果也无明显差异,是一种安全、简便的诊断手段,对于急诊检验血糖具有十分重要的意义,受到了患者家属的普遍好评,值得在临床中大力推广。     

固相微萃取GC-MS法分析水中的香料

固相微萃取是1种可取代常规样品提取方法的快速、而又无需溶剂的样品提取技术.本文采用固相微萃取(SPME)技术与GC-MS技术成功地对水中的香料进行快速分析,所得出的结果快速、准确,方法与常规方法相比具有省时、灵敏度高、无需萃取溶剂的独特优点.     

光度法快速分析苯乙酮酸含量的研究

研究了一种快速定量分析发酵液中苯乙酮酸的方法。在氢氧化钠溶液中,苯乙酮酸和2,4-二硝基苯肼形成一种红棕色的溶液,该溶液在458 nm处有最大吸收,据此可以快速分析混合物中苯乙酮酸的含量。该法在微生物还原苯乙酮酸生产D-扁桃酸的工艺中进行样品分析,结果表明方法简便、快速、灵敏度高,可以用于监控反应进程。     

桑色素极谱行为的研究

研究了桑色素在pH=1～14的水溶液中的极谱行为. 于不同pH范翻内得列了四个还原波. 研究证实在pH<4条件下获得的P_1波为表面催化氢波. 其余三个波为不同形态桑色素的单电子吸附还原波, 并伴有随后化学反应过程. 测得在单分子层饱和吸附条件下, 每一个桑色素分子所占汞电极面积为1.36 nm.     

The flat surfaced membrane coated mercury electrode as analytical tool in the continuous voltammetric analysis

Specific analytical problems often arise which can be easily solved if a mercury electrode of constant surface area is used as voltammetric sensor. In this work a membrane covered mercury electrode was prepared and used in solving various analytical tasks. One of them was the determination of water hardness. A sample injection method was developed applying EDTA reagent and a flow-through analytical system. Two different voltammetric enzyme electrodes (measuring glucose and L-amino acid) were prepared by using the membrane covered mercury electrode as base sensor. The application of the enzyme electrode in flow-through circumstances was proved to be very advantageous in determining selectively L-DOPA in the presence of the D-form.     

巯基—聚吡咯薄膜修饰电极的制备及其电化学性能

通过将巯基乙酸作为一种支持电解质,将巯基固定在导电聚吡咯薄膜电极上,从而制得巯基—聚吡咯薄膜修饰电极,该修饰电极保持了巯基的螯合性能,并具有良好的稳定性。对水溶液中的重金属离子具有很好的吸附作用,其灵敏度与未修饰的玻碳电极相比,测汞离子时电沉积提高了3倍,化学吸附时提高了近5倍。并对其吸附机理进行了初步的探讨,证明了其对汞离子的吸附为不可逆的产物弱吸附。     

High flow-rate cells for continuous monitoring of low concentrations of electroactive species by polarography and stripping voltammetry at the static mercury drop electrode

A high-capacity flow-through cell which can be used at a maximum flow rate of 300 ml min^-1 has been developed for continuous monitoring of electroactive substances. The cell is compatible with the recently developed static mercury drop electrode. Comparative studies with a cell employing a conventional dropping mercury electrode are described. A wide range of polarographic techniques is applied, and it is demonstrated that the static mercury drop electrode improves the limits of detection, that laminar flow conditions are essential for low noise levels of operation, and that solution flow through a sulphite bed is a more effective method of oxygen removal than nitrogen bubbling. The combination of a microprocessor-controlled polarographic system, static mercury drop electrode and high-volume flow cell is very versatile for the determination of trace levels of electroactive species in flow streams. Preliminary results on anodic stripping voltammetry in flow streams are reported.     

单扫描示波极谱法同时测定水样中锌铁锰

探讨以固体电极代替滴汞电极作工作电极,用示波极谱法同时测定微量元素,在环境监测分析中的应用,试验表明,方法操作简便,快速,直观,地毒,无污染,而且稳定性和重现性较好,可以推广应用。     

Electrodeposition of mercury on gold from very dilute mercury(II) solution

Flameless atomic absorption spectrometry (flameless a.a.s.) was applied to study the state of mercury deposited on a gold plate electrode from very dilute mercury(II) solution by controlled-potential electrolysis. A stable monolayer is formed on the gold electrode by the electrolysis at a potential about 200 mV more positive than the reversible Nernst potential for the reduction of mercury(II) to mercury(0). After the monolayer formation, bulk mercury is deposited on the monolayer at the reversible potential and an adatom layer is also found. The difference of activation free energies between the evaporation of mercury from the monolayer and that from bulk mercury corresponds to the underpotential shift for the electrodeposition of mercury on the gold electrode.     

Voltammetric quantification and speciation of mercury compounds

The use of a carbon paste electrode modified with a thiolic resin for the determination of inorganic mercury and organomercury compounds, present simultaneously in a sample, is described. The compounds are first preconcentrated at the electrode surface by means of a purely chemical reaction with the modifier on the electrode surface. The high affinity of the modifier for the mercury compounds ensures low limits of detection and determination. Differentiation between several mercury species is possible by control of the reduction potential applied to the working electrode. This selective reduction results in the formation of atomic mercury at the electrode surface which can be determined with a very high sensitivity by means of its re-oxidation wave in cyclic voltammetry. Optimization of the instrumental parameters and evidence for the reduction processes are discussed. Analysis of inorganic mercury in the presence of methylmercury, with a detection limit of 4 μg Hg 1⁻¹, and of methylmercury in the presence of inorganic mercury, with a detection limit of 2 μg Hg 1⁻¹, is described in detail. In both cases the preconcentration time is 6 min. Other organomercury species can also be quantified. Application of the method to environmental aquatic samples is discussed.     

Voltammetric methods for determination of mercury in domestic waste and compost

A voltammetric method for the determination of mercury in domestic waste, compost produced from it and in water extracts of these samples is described. The solid samples have been digested with concentrated acids and the extracts by UV irradiation. Conditions for the voltammetric determination of mercury with a gold disc electrode in samples of very complicated composition have been worked out. To avoid the disturbing influence of copper a special potential — time program has been applied, whereas the disturbing effect of iron has been removed by complexation of Fe(III) with fluoride ions or by medium exchange. The procedure proposed suits very well for determination of mercury in the samples studied. A very low leachability of mercury from compost was found.     

Voltammetric analysis of ceftazidime after preconcentration at various mercury and carbon electrodes: application to sub-ppb level determination in urine samples

The electrochemical behavior of ceftazidime (CFZ) at four different kinds of electrodes viz. static mercury drop electrode (SMDE), controlled growth mercury electrode (CGME), glassy carbon electrode (GCE) and carbon paste electrode (CPE) has been presented. Optimal operational parameters have been selected for the drug preconcentration and determination in aqueous medium. Down to 2x10(-10) M CFZ is achieved as detection limit at the CGME. Modification of the CPE with polyvinyl alcohol (PVA) enhances both the sensitivity and selectivity for the drug accumulation and, therefore, its determination at very low levels. Application of the proposed method for CFZ analysis in spiked urine samples or those taken after metabolism has been easily assessed. Down to 1x10(-9) M CFZ (0.695 ng ml(-1)) could be easily achieved in such samples.     

石墨电极的纯度对直读光谱分析的影响

石墨电极的纯度对光谱分析的影响只是在一些书中提及,表作试验研究和分析,对电极的纯度的检验未作有效论述。文中就此问题提出了作者的见解,拟定了检验电极纯度的方法。