A benzenesulfonic acid-modified organic polymer monolithic column with reversed-phase/hydrophilic bifunctional selectivity for capillary electrochromatography

Here,a styrene-based polymer monolithic column poly(VBS-co-TAT-co-AHM)with reversed-phase/hydrophilic interaction liquid chromatography(RPLC/HILIC)bifunctional separation mode was success-fully prepared for capillary electrochromatography by the in situ polymerization of sodium p-styrene sulfonate(VBS)with cross-linkers 3-(acryloyloxy)-2-hydroxypropyl methacrylate(AHM)and 1,3,5-triacryloylhexahydro-1,3,5-triazine(TAT).The preparation conditions of the monolith were optimized.The morphology and formation of the poly(VBS-co-TAT-co-AHM)monolith were confirmed by scanning electron microscopy(SEM)and Fourier transform infrared spectroscopy(FT-IR).The separation perfor-mances of the monolith were evaluated systematically.It should be noted that the incorporation of VBS functional monomer can provideπ-πinteractions,hydrophilic interactions,and ion-exchange in-teractions.Hence,the prepared poly(VBS-co-TAT-co-AHM)monolith can achieve efficient separation of thiourea compounds,benzene series,phenol compounds,aniline compounds and sulfonamides in RPLC or HILIC separation mode.The largest theoretical plate number for N,N0-dimethylthiourea reached 1.7×10^(5)plates/m.In addition,the poly(VBS-co-TAT-co-AHM)monolithic column showed excellent reproducibility and stability.This novel monolithic column has great application value and potential in capillary electrochromatography(CEC).

Capillary Electrochromatography Using C_8 Open Tubular Column Prepared by Sol-Gel Technique

Open tubthar C8 columns were prepared by sol-gel technology and used in the electrochromatographic separations.

Determination of Five Organic Acids in Radix Isatidis by Column Partition Chromatography and Capillary Zone Electrophoresis柱分配色谱-毛细管区带电泳联用分析板蓝根中五种微量有机酸(英文)

Aim To determine five organic acids in Radix Isatidis . Method The extraction method and the column partition chromatographic conditions were studied. Then a capillary zone electrophoretic method was set up for the determination. Results The linear ranges of quinazolinone acid, n anthranilic acid, benzoic acid, salicylic acid, and syringic acid were 5 52-92 0 μg·mL -1 , 5 12-102 μg·mL -1 , 2 28-84 4 μg·mL-1 , 4 78-159 μg·mL -1 , and 1 74-87 0 μg·mL -1 respectively. Conclusion The established method is accurate and simple.

Separation of Inorganic Anions Using Methacrylate-Based Monolithic Column Modified with Trimethylamine in Ion Chromatography Capillary System

Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.

THE SEPARATIONS OF ENANTIOMERS OF α—SUBSTITUTED-(2—PYRIDYL)—METHYLAMINES ON A CHIRASIL-VAL CAPILLARY COLUMN

Enantiomers of a-substituted-(2-pyridyl)-methylarfdnes uere separated on SC -7 gas chromatograph with a 20m×0.25mm Chirasil-Val capIlary column,Carrier gas was nitro- gen or hydrogen.The resolution factors(ri.s) were 1.02 to 1.06.Enantiomers of pyridyl anines were separated to and near to base line.

Evaluation of the Equality of Non-Polar Capillary Columns in GC/MS Analysis of Food Contact Plastics

Non-polar capillary columns for GC/MS are widely utilized in the analysis of additives for food contact materials. Though various kinds of non-polar capillary columns are commercially available, the equality of their performance has not been verified. Herein, ninety-six additives for food contact plastics were analyzed using fifteen kinds of columns, and the peak separation, retention times, and peak areas of each additive were compared. The additives, with various chemical properties, comprised forty four plasticizers, twenty lubricants, twenty antioxidants, nine ultraviolet absorbers, and three other compounds. 10 μg.mL-1 test solutions were prepared in acetone, and injected to the GC/MS. The fifteen columns were classified into five categories based on the chromatogram pattern and peak separation. To facilitate comparison of the retention time and detection sensitivity of the columns for the additives, the relative retention time (RRT) and relative peak area (RPA) were calculated by using dibutylphthalate or 4-tert-butylphenylsalicylate as an internal standard. The RRTs of the additives on each column were essentially similar. However, the RRT of the additives which were detected in the later stages differed slightly. Although the RPA of the plasticizers and lubricants were roughly similar, column-to-column differences were observed for certain additives, such as antioxidants and ultraviolet absorbers. Furthermore, certain fatty acids, antioxidants, two plasticizers, and two benzophenone type ultraviolet absorbers were not detected in the chromatograms of two columns.

Capillary Zone Electrophoretic Separation of Basic Proteins with Coated Columns Prepared by Sol-Gel Technology

Coated capillary columns were prepared by sol-gel technology and used in the separation of basic proteins with capillary zone electrophoresis. The results indicated that a significant decrease in protein adsorption was obtained and EOF was also diminished to zero in the pH range of 3-10.

AN EASY-TO-MAKE OZONE GENERATOR FOR THE IMMOBILIZATION OF STATIONARY PHASES IN GC CAPILLARY COLUMNS

An easy-to-make ozone generator which can be made with readily available materials is proposed. Concentration of the ozone prepared with this generator could reach that of ozone in equilibrium with oxygen. Cured with the ozone thus prepared, GC capillary columns with immobilized SE-54 phase and excellent chromatographic performance were successfully prepared.

CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF 3-PHENYL-1,2-EPOXYETHANE AND 1-PHENYL-1-PROPANOL ON A FUSED SILICA CAPILLARY COLUMN COATED WITH PERBENZYL-β-CYCLODEXTRIN

A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.

毛细管顶空气相色谱法高灵敏监测花生大豆根瘤生物固氮能力

建立了测定花生和大豆根瘤菌生物固氮能力的毛细管顶空气相色谱法,利用固氮酶还原乙炔气体为乙烯的经典方法,实现了高浓度乙炔中痕量乙烯的高灵敏分析。利用顶空进样方式,分离柱采用HP-PLOT Q毛细管色谱柱,程序升温,采用氢离子化检测器,对乙烯标准气体进行了定量分析。乙烯检测范围宽为0.125~30000μmol/mol,相关系数为0.9996,检测限(LOD)为0.0341μmol/mol,检出限优于已有报道。该方法检测精密度好,5次检测的相对标准偏差为2.32%。乙烯样品的回收率为95.8%~110%,相对标准偏差为1.54%~3.47%。同时,对乙烯和实际样品进行检测时,与GDX-502填充柱的传统气相色谱法的测定结果一致,表明所建立的乙烯顶空气相色谱法具有较高的可靠性。此外,该方法分析时间缩短至3 min,利用自动进样方式,检测通量大,适用于花生和大豆根瘤菌中固氮能力的快速准确测定,能满足花生和大豆生物固氮研究中乙炔还原法测定乙烯的需求。

深小孔电解加工阴极侧壁绝缘层制备及试验

航空发动机零部件中存在大量深小孔,不仅孔径小、深径比大,而且要求孔表面没有再铸层,这些特点给孔的加工带来了很多困难。电解加工是一种有效的加工方法,针对大深径比小孔电解加工所用的阴极侧壁绝缘层制备困难,且使用过程中容易损坏的问题,尝试了多种材料、多种方式的绝缘层制备方法,并对其在加工过程中的性能稳定性进行了试验研究,最终提出了一种基于弹性石英毛细管的新型多层复合绝缘层制备方法,并借助该方法制作管阴极,在不锈钢材料上成功加工出直径1.1 mm、深径比达181的深小孔。

SPME-气相色谱串联质谱法检测食品中的环氧乙烷及其代谢物2-氯乙醇

建立了顶空固相微萃取(solid phase micro extraction,SPME)-气相色谱串联质谱(GC-MS/MS)法检测食品中的环氧乙烷及其代谢物2-氯乙醇的分析方法。样品采用SPME(萃取纤维头95umC-WR/PDMS)在线提取,使用毛细管色谱柱HP-VOC分离环氧乙烷和2氯乙醇及其他干扰组分,高效电子轰击电离源(HES)离子化,多反应监测(multiple reaction monitoring,MRM)扫描,外标法定量。环氧乙烷及2-氯乙醇在10~200μg/L线性范围内,线性关系良好(r>0.995),以环氧乙烷表示的环氧乙烷和2氯乙醇的总和方法定量限20μg/kg,在1倍、2倍和10倍定量限3个浓度添加水平下,水果、蔬菜、谷物及调味料食品中添加回收率在76.32%~102.05%之间,重复性精密度在1.66%~5.96%之间。该方法灵敏度高、准确度高、重现性好,适用于食品中环氧乙烷及其代谢物2-氯乙醇的检测。

气相色谱毛细管柱的选择

气相色谱已成为石油化工中重要的分析方法,在研究挥发性与半挥发性成分时发挥着重要的作用,对于常规的应用和研究都具有重要的意义。而气相色谱柱是气相色谱的核心。选择合适的色谱柱可以改善色谱分离结果,快速提高实验效率。本文从固定相、柱内径、膜厚、柱长与相位比(β)等多个角度描述色谱分离的基本原理,介绍选择毛细管色谱柱的相关概念,供相关实验人员参考。

MIL-101(Cr)在气体分离方面的应用

以金属有机框架材料MIL-101(Cr)作为气相色谱固定相,分别制作了毛细管柱和不锈钢填充柱,用来分离可燃气体。首先合成MIL-101(Cr),将该材料制成60~100目的颗粒,抽入2 m的不锈钢填充柱内,老化后接入气相色谱。在一定的条件下该色谱柱可以分离氮气、一氧化碳、甲烷、二氧化碳、乙烷、乙烯、乙炔,且出峰时间短,柱效与分离度都可以满足日常使用的需求。将合成的MIL-101(Cr)与二氯甲烷混合制成悬浊液,用动态涂渍法涂渍到一根15 m的毛细管柱内,老化色谱柱,然后接入气相色谱内,按照设定好的条件分离烃类。实验证明,该毛细管柱可以分离部分烃类。

Advances in capillary electro-chromatography

Capillary electrochromatography (CEC) is a micro-scale separation technique which is a hybrid between capillary electrophoresis (CE) and liquid chromatography (LC). CEC can be performed in packed, monolithic and open-tubular columns. In recent three years (from 2016 to 2018), enormous attention for CEC has been the development of novel stationary phases. This review mainly covers the development of novel stationary phases for open-tubular and monolithic columns. In particular, some biomaterials attracted increasing interest. There are no significant breakthroughs in technology and principles in CEC. The typical CEC applications, especially chiral separations are described.

Drainage performance and capillary rise restraint effect of wicking geotextile

Wicking geotextile(WG)is considered as a possible countermeasure to reduce water content in unsaturated soil.In this research,rainfall tests were carried out to verify the drainage performance of WG.And capillary rise tests were conducted to study the effect of WG on the prevention of capillary rise.Test results indicated that WG with good drainage performance could drain gravitational and capillary water out of kaolinite soil.For kaolinite soil column with water content of 12%and compaction degree of 90%,the whole process of capillary rise in soil column with a layer of WG was a typical two-stage mode,and the maximum capillary height was about 380 mm,which provided that the WG could work as a barrier to prevent capillary rise effectively.In addition,the total vertical influential regions of WG in kaolinite soil above and below the WG layer were 400 and 100 mm,respectively.

Advances in Capillary Chromatography

Capillary columns are used in both capillary liquid chromatography and capillary electrochromatography. The design for capillary liquid chromatography is discussed in comparison with capillary gas chromatography. The difference of diffusion coefficient in gas and liquid phase is a key role. The study for obtaining a high performance capillary liquid chromatography is discussed. Capillary electrochromatography is recently interesting for its instinct ability to realize a high performance chromatography. Capillary electrochromatography with and without pressurized flow is reviewed briefly. Instrumentation for capillary electrochromatography with pressurized flow is discussed. The port of splitting, and gradient elution of both solution and potential are described. The new findings of both the variation of column resistance and capacity factor according to the value of applied electric voltage are also discussed.

Preparation and Application of an Immunoaffinity Column for Direct Extraction of Morphine and its Analogs from Opium

A rapid, simple and accurate method using an immunoaffinity column (IAC) and capillary electrophoresis (CE) for the analysis of the major alkaloids in opium is developed. The IAC was synthesized by coupling specific morphine polyclonal antibodies to CNBr-actived Sepharose 4B. The IAC showed high selectivity and obvious enrichment to morphine, codeine, dionin and thebaine. The extraction solution was analyzed by CE with β-cyclodextrin as an additive. Recoveries of the four alkaloids from PBS were between 93%-105% with RSD value less than 5.0%. The result showed that this method was practical for the determination of morphine analogs in opium.

潜水矿化度对毛细水上升高度的制约特征研究

为了探究不同土壤类型矿化度对毛细水上升高度的制约特征,文章选取不同粒径砂性土与砂质壤土开展不同矿化度影响下的土壤毛细水室内柱试验研究,定量刻画了粒径与矿化度对毛细水上升高度的差异,建立了对数函数拟合模型。试验结果表明,矿化度通过改变土壤水的重力势、基质势来制约毛细水的上升高度。矿化度为0.8、15.0、50.0g/L时,72 h中砂最大毛细水上升高度h_(max)分别为32.5、31.3、30.2 cm,细砂h_(max)分别为50.4、48.6、48.7 cm,粉砂h_(max)分别为72.3、76.4、76.0 cm,砂质壤土h_(max)分别为59.0、60.2、58.6 cm;粉砂和砂质壤土的毛细水上升速率变化波动较大,全试验周期内毛细水上升高度h与时间t可用三参数对数函数刻画。该研究结果揭示了矿化度对毛细水上升高度的制约特征,深化了毛细水上升高度的机理研究,可为土壤盐渍化治理、确定地下水生态水位提供技术支撑。

顶空进样毛细柱气相色谱法检测水中三氯甲烷研究

采用顶空气相色谱法检测水中三氯甲烷的质量浓度,毛细管色谱柱为HP-5,检测器为电子捕获检测器(ECD)。实验结果表明:三氯甲烷的线性范围为0~60.0μg/L,相关因子为0.9995;精密度为2.8%~4.3%;加标回收率91.8%~104.0%;检出限为0.2μg/L。该方法简便、快速,具有较好的精密度与准确度,可用于水中三氯甲烷的测定。