Recent trends in capillary and micro-chip electrophoretic instrumentation for field-analysis

Technical advances in the development of field-deployable capillary and microchip electrophoretic instruments and reports of their deployment between 2013 and 2017 were reviewed. Strategies and considerations in the design of the injection, separation and detection hardware, chemistry and associated infrastructure were discussed from an in-field perspective, with portability, robustness and automation/“ease of use” featuring as key requirements. Integration of functionality is important for adequate in-field performance. Progress was made towards the use of multiple channel devices for increased throughput and/or resolving power, mixing devices for on-line/in-line sample derivatization, battery operation and temperature control. The strengths and weaknesses of the various approaches described in the literature are discussed from the perspective of in-field operation. An overview of the applications of the field electrophoretic instruments is provided, including environmental science and planetary investigation.     

Determination of vitamin C and preservatives in beverages by conventional capillary electrophoresis and microchip electrophoresis with capacitively coupled contactless conductivity detection

The separation and detection of commonly used preservatives (benzoate, sorbate) and vitamin C by both conventional CE and microchip electrophoresis with capacitively coupled contactless conductivity detection is presented. The separation was optimized by adjusting the pH-value of the buffer and the use of hydroxypropyl-beta-CD (HP-beta-CD) and CTAB as additives. For conventional CE, optimal separation conditions were achieved in a histidine/tartrate buffer at pH 6.5, containing 0.025% HP-beta-CD and 0.1 mM CTAB. LOD ranged from 0.5 to 3 mg/L (S/N = 3) and the RSDs for migration time and peak area were less than 0.1 and 2%, respectively. A considerable reduction of analysis time can be accomplished by using microchip electrophoresis without significant loss in sensitivity under optimal separation conditions. A histidine/tartrate buffer at pH 6.5, incorporating 0.06% HP-beta-CD and 0.25 mM CTAB, gave detection limits ranging between 3 and 10 mg/L and satisfactory reproducibilities of < or =0.4% for the migration time and < or =3.5% for the peak area. The methods developed are useful for the quantitative determination of food additives in real samples such as soft drinks and vitamin C tablets.     

Automated capillary electrophoresis with on-line preconcentration by solid phase extraction using a sequential injection manifold and contactless conductivity detection

An extension of a capillary electrophoresis instrument coupled to a sequential injection analysis manifold was developed for automated measurements with on-line solid-phase extraction preconcentration. An in-house built capacitively coupled contactless conductivity detector was employed for sensitive detection with narrow capillaries of 25 μm internal diameter. The system was assembled into standardized 19 in. frames and racks for easy transport and mobile deployment. The system can be left running unattendedly without manual intervention with good operation stability. To demonstrate the application of the system, a method for the determination of four drugs, namely ibuprofen, diclofenac, naproxen and bezafibrate, was developed with enrichment factors of up to several hundreds. Detection of the drug residues down to the nM-scale was found possible and the method was found suitable for the detection of ibuprofen in the waste water of a hospital in Hanoi.     

Electronic technique and circuit topology for accurate distance-independent contactless readout of passive LC sensors

Contactless readout of passive LC sensors composed of a capacitance sensor connected to a coil can be performed through a readout coil electromagnetically coupled with the sensor coil. Resonant frequency and quality factor can be extracted from the impedance measured at the readout coil by a technique which results theoretically independent of the coupling, and, therefore, the distance between the readout and the sensor coils. However, the effect of the unavoidable parasitic capacitance connected to the readout coil introduces in practice an undesired dependence of the measured values on the distance between the coils, resulting in a decreased accuracy. In this paper, such dependence is predicted by the results of a numerical analysis and experimentally verified. To overcome this limitation, a novel electronic technique and circuit topology for the compensation of the readout parasitic capacitance is proposed. The experimental results show that the compensation technique allows to read the resonant frequency of a LC pair at around 5.3 MHz with a variation of less than 200 ppm across an interrogation distance between 2 and 24 mm.     

针对EMVLevel1 Analog Test认证的金融支付PCD设计与调试

文章针对最新版EMV Level 1标准,对PCD的EMV Level 1 Analog test认证的检测环境及检测项目进行总结,对实际测试中可能遇到的问题进行分析,总结出其技术难点。针对这些难点提出PCD设计中需要重点关注的方面以及设计技巧,进一步给出调试中使用怎样的方法达到系统的最优配置,成功通过EMV Level1 Analog test的检测。     

Capillary electrophoresis for the analysis of paralytic shellfish poisoning toxins in shellfish: Comparison of detection methods

Paralytic shellfish toxins (PSTs) are produced by marine and freshwater microalgae and accumulate in shellfish including mussels, oysters, and scallops, causing possible fatalities when inadvertently consumed. Monitoring of PST content of shellfish is therefore important for food safety, with currently approved methods based on HPLC, using pre‐ or postcolumn oxidation for fluorescence detection (HPLC‐FLD). CE is an attractive alternative for screening and detection of PSTs as it is compatible with miniaturization and could be implemented in portable instrumentation for on‐site monitoring. In this study, CE methods were developed for C⁴D, FLD, UV absorption detection, and MS—making this first report of C⁴D and FLD for PSTs detection. Because most oxidized toxins are neutral, MEKC was used in combination with FLD. The developed CZE‐UV and CZE‐C⁴D methods provide better resolution, selectivity, and separation efficiency compared to CZE‐MS and MEKC‐FLD. The sensitivity of the CZE‐C⁴D and MEKC‐FLD methods was superior to UV and MS, with LOD values ranging from 140 to 715 ng/mL for CZE‐C⁴D and 60.9 to 104 ng/mL for MEKC‐FLD. With the regulatory limit for shellfish samples of 800 ng/mL, the CZE‐C⁴D and MEKC‐FLD methods were evaluated for the screening and detection of PSTs in shellfish samples. While the CZE‐C⁴D method suffered from significant interferences from the shellfish matrix, MEKC‐FLD was successfully used for PST screening of a periodate‐oxidized mussel sample, with results confirmed by HPLC‐FLD. This confirms the potential of MEKC‐FLD for screening of PSTs in shellfish samples.     

Monitoring of amoxicilline and ceftazidime in the microdialysate of diabetic foot and serum by capillary electrophoresis with contactless conductivity detection

Determination of the broad-spectrum antibiotics amoxicilline (AMX) and ceftazidime (CTZ) in blood serum and microdialysates of the subcutaneous tissue of the lower limbs is performed using CE with contactless conductivity detection (C⁴D). Baseline separation of AMX is achieved in 0.5 M acetic acid as the background electrolyte and separation of CTZ in 3.2 M acetic acid with addition of 13% v/v methanol. The CE-C⁴D determination is performed in a 25 µm capillary with suppression of the EOF using INST-coating on an effective length of 18 cm and the attained migration time is 4.2 min for AMX and 4.4 min for CTZ. The analysis was performed using 20 µl of serum and 15 µl of microdialysate, treated by the addition of acetonitrile in a ratio of 1/3 v/v and the sample is injected into the capillary using the large volume sample stacking technique. The LOQ attained in the microdialysate is 148 ng/ml for AMX and 339 ng/ml for CTZ, and in serum 143 ng/ml for AMX and 318 ng/ml for CTZ. The CE-C⁴D method is employed for monitoring the passage of AMX and CTZ from the blood circulatory system into the subcutaneous tissue at the sites of diabetic ulceration in patients suffering from diabetic foot syndrome and also for measuring the pharmacokinetics following intravenous application of bolus antibiotic doses.     

液液萃取-场放大进样-毛细管电泳非接触式电导分离检测酱油中的安赛蜜

采用场放大进样（FASI）-毛细管电泳非接触式电导检测法（CE-C⁴D）,结合液液萃取（LLE）的样品净化预处理技术,分离检测了酱油中人工合成甜味剂安赛蜜。酱油样品经酸化后,用乙酸乙酯作为萃取剂,成功地消除了酱油中含有的大量无机盐等复杂基体对微量安赛蜜的干扰。实验对影响LLE萃取效率和FASI-CE-C⁴D分离检测的关键因素进行了讨论,特别是对样品净化前处理过程中萃取剂及用量、样品酸化pH值、萃取时间、萃取温度等条件进行了优化。结果表明,酱油中的安赛蜜可获得良好分离和灵敏检测,检出限和定量限分别为0.15 mg/kg和0.48 mg/kg。对市售酱油样品进行安赛蜜的加标回收测定,得到加标回收率为92.3%~108.1%,相对标准偏差＜8.0%。该法具有简单快速、灵敏高效、分析成本低的优点,能满足酱油中安赛蜜的分析检测要求。     

毛细管电泳及芯片毛细管电泳的电容耦合非接触电导检测

综述了毛细管电泳(CE)及芯片毛细管电泳(MCE)的电容耦合非接触电导检测(Capacitively Coupled Contactless Conductivity detection,C4D)的研究状况;并分别对其装置、检测的影响因素及其应用进行了评述。引用文献81篇。     

微流控芯片测定盐酸金刚烷胺片中的盐酸金刚烷胺

建立了微流控芯片非接触电导检测片剂中盐酸金刚烷胺的分析方法.对缓冲液和添加剂的种类及浓度、分离电压、进样时间等进行了优化.实验采用1 mmol/L HAc+2 mmol/L NaAc(pH 4.5)+0.1 mmol/LSDS的缓冲体系,于2.00kV的分离电压下进样10 s,在1 min内实现了盐酸金刚烷胺的快速检测...