反相硅胶整体柱离子色谱法快速分析BrO-3

研究了基于反相硅胶整体柱的离子色谱快速分析BrO;的方法.以氢氧化四丁铵(TBA)为流动相动态修饰反相硅胶整体柱,采用直接电导检测,在普通高效液相色谱仪上实现了BrO3-和常见阴离子的快速分析.实验考察并讨论了流动相、色谱柱温度和流速对所测阴离子保留和分离的影响.确定分离测定BrO3-的最佳色谱条件是:以0.75 mm...     

表面接枝型离子色谱固定相的制备

以苯乙烯-二乙烯基苯微球为基质,建立了一种新型离子色谱固定相的制备方法。在基质微球表面合成一层聚缩水甘油甲基丙烯酸酯聚合物层(GMA),随后与甲胺及1,4-丁二醇二环氧甘油醚(BDDE)交替反应,与其表面接枝上带正电荷的季铵基团,可用于阴离子的分离。通过改变接枝反应的次数,控制交换树脂的交换容量。自制色谱固定相能够用于7种常规阴离子分离分析,并用于自来水中常规阴离子的检测。分离检测结果可与商用离子色谱柱相比,同时水负峰能与氟离子完全分离,不影响氟离子的定量检测。     

弱阴离子交换整体柱对白介素-18的分离

制备了弱阴离子交换整体柱,并建立了白介素-18在该柱上分离纯化的方法。以色谱柱管为模具,通过原位聚合法制备了一种以甲基丙烯酸缩水甘油酯(GMA)为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂的整体色谱柱,并用二乙胺将其修饰为弱阴离子交换柱。考察了交联剂及致孔剂用量对色谱柱压力的影响,发现:随着交联剂用量的减小,致孔剂用量的增大,柱压下降;当交联剂和致孔剂用量达到一定水平后,柱压变化不再明显,但柱体机械强度降低。用该柱对白介素-18进行了分离,同时考察了不同固定相、缓冲液体系、pH值、盐的类型以及有机添加剂对白介素-18分离效果的影响。方法简单、灵敏、快速,重现性好。     

柱切换离子色谱法测定丙酮中痕量阴离子

建立了测定丙酮中痕量阴离子的离子色谱分析方法.采用的是高效液相柱切换进样,其中泵的流速为0.5 mL/min,使低浓度的丙酮水溶液在保护柱上富集,通过离子色谱抑制电导法分离和检测丙酮样品中痕量的阴离子.色谱条件为:以IonPacAG9-HC(50 mm×2 mm)型柱串联在定量环中进行富集,IonPacAG9-HC(50 mm×2 mm)保护柱,IonPac AS9-HC(250 mm×2 mm)阴离子分离柱进行分离,流动相为9 mmol/L Na2CO3-1.667 mol/L NaHCO3,所得回收率在96.21%～101.56%之间,线性良好,且具有较好的重现性和较低的检出限.     

离子色谱法测定化肥中六种阴离子

提出了离子色谱法同时测定化肥中6种无机阴离子的方法。化肥试样经水超声浸取,采用C18固相萃取柱和Ba固相萃取柱净化,萃取液中氟离子、氯离子、亚硝酸根、溴离子、碘离子、硫氰酸根以IonPac AS18(250 mm×4 mm)为分析柱、IonPac AG18(50 mm×4 mm)为保护柱,氢氧化钾溶液梯度洗脱分离并用电导检测器同时测定了6种阴离子的含量。6种阴离子的检出限(3S/N)在0.001 2~0.013 5 mg.L-1之间。方法的加标回收率在78.9%~103.0%之间,相对标准偏差(n=6)在0.61%~6.5%之间。     

离子色谱同时分离测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子

建立了离子色谱-直接电导检测同时测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子(F-,Cl-,Br-,NO3-,SO24-)的方法。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用对羟基苯甲酸-三(羟甲基)氨基甲烷-硼酸,邻苯二甲酸-三(羟甲基)氨基甲烷,邻苯二甲酸氢钾为淋洗液,考察了淋洗液种类,浓度及色谱柱温度对分离测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子的影响。最佳色谱条件为:以1.2mmol/L邻苯二甲酸氢钾为淋洗液,柱温30℃,流速1.0mL/min。在此条件下,可同时基线分离7种阴离子,且色谱峰形对称。所测阴离子的检出限(S/N=3)为0.02～1.88mg/L,保留时间和峰面积的相对标准偏差(n=5)分别小于0.17%和2.05%。应用本方法测定离子液体中三氟甲烷磺酸根,氟硼酸根及常见无机阴离子,加标回收率在97.0%～102.8%之间。本方法简单,准确,可靠,具有较好的实用性。     

聚苯胺/石墨烯涂覆型阴离子交换固定相的制备及表征

该文以聚苯胺/石墨烯复合材料为涂覆材料,制备了一种涂覆型阴离子交换固定相。首先以苯胺和石墨烯为原料制备聚苯胺/石墨烯复合材料,并通过物理吸附涂覆在聚苯乙烯-二乙烯苯微球表面;然后以聚苯胺中的氮原子为反应位点,通过季铵化制备一系列具有不同交换容量的涂覆型阴离子交换固定相。通过扫描电镜(SEM)、傅里叶红外光谱(FT-IR)和元素分析(EA)对该涂覆型阴离子交换固定相进行表征,结果表明聚苯胺/石墨烯成功地涂覆在微球表面且发生了季铵化。通过分离常规阴离子和有机酸,对自制阴离子交换色谱柱的色谱性能进行评价。结果显示,8次季铵化的聚苯胺/石墨烯涂覆聚苯乙烯-二乙烯苯阴离子交换色谱柱对常规阴离子和有机酸呈现良好的分离效果。     

氧化银作沉淀剂消除基体中氯离子干扰的离子色谱方法

1 引言 大量氯离子的存在对离子色谱阴离子分析干扰是离子色谱阴离子分析的较常见的问题.目前,离子色谱阴离子分析中去掉基体中大量氯离子最有效的方法为银柱法,此法将含有高氯离子浓度的溶液流过高容量银型阳离子交换柱,溶液中与氯离子对应的阳离子会置换一些阳离子交换柱上的银离子,交换下来的银离子和溶液中的氯离子形成沉淀从而排除了氯离子的干扰.由于沉淀生成在银柱内,需经常清洗,柱子的使用寿命较短.本实验采用固体氧化银作为沉淀剂,用氧化银溶解出的浓度非常低的银离子与氯离子产生沉淀,排除氯离子干扰.本实验研究了处理条件以及处理方法对与银离子的溶度积非常小的铬酸根、草酸根、磷酸根的检测的影响,用此法分析了分析纯氯化物试剂中的微量阴离子.     

超支化修饰亲水型阴离子色谱柱的制备与应用

超支化树状修饰方法凭借灵活、可控的结构设计,在聚合物基固定相的疏水改性中发挥着重要作用。该文以聚苯乙烯-二乙烯基苯为基质微球,1,4-丁二醇二缩水甘油醚、四乙烯五胺为环氧-胺接枝原料,以甲胺封端,制备了亲水型离子色谱固定相。利用扫描电子显微镜(SEM)、比表面积分析仪(BET)、傅里叶红外光谱仪(FTIR)、X射线光电子能谱仪(XPS)分析固定相的形貌、结构和表面元素。随后将固定相填充成色谱柱,以无机阴离子、有机弱酸为分离目标评价色谱柱的分离性能和保留机制,计算目标离子的分离度和理论塔板数。通过改变淋洗液浓度、温度和种类,考察自制色谱柱的保留行为和分离性能。结果表明,采用环氧-胺树状支化的修饰方式引入羟基,可有效增加固定相的亲水性。二价离子(SO₄^2-、HPO₄^2-)受影响较大,表现出弱保留行为,而低价离子为离子交换保留行为。在3.6 mmol/L Na₂CO₃淋洗液条件下,制备的色谱柱可在20 min内完成12种阴离子(F^-、CH<...     

直接电导检测-离子色谱法分离测定氟硼酸根及常见无机阴离子

研究了直接电导检测-离子色谱法分离测定BF4-及常见无机阴离子(F-、Cl-、Br-、NO3-、SO24-)。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用邻苯二甲酸氢钾、对羟基苯甲酸 三(羟甲基)氨基甲烷 硼酸、邻苯二甲酸 三(羟甲基)氨基甲烷为淋洗液,考察了淋洗液种类、浓度、色谱柱温度、流速对分离测定BF4-及常见无机阴离子的影响。确定最佳色谱条件为:以1.25 mmol/L邻苯二甲酸氢钾为淋洗液,流速1.5 mL/min,柱温45℃。在此条件下可同时基线分离6种阴离子,且色谱峰形对称。所测阴离子的检出限为0.02~0.58 mg/L;峰面积的相对标准偏差(RSD,n=5)小于0.8%。将方法应用于测定离子液体中的BF4-及其它无机阴离子,加标回收率在98.2%~102.7%之间。     

Macroporous poly(glycidyl methacrylate-triallyl isocyanurate-divinylbenzene) matrix as an anion-exchange resin for protein adsorption.

A novel macroporous poly(glycidyl methacrylate-triallyl isocyanurate-divinylbenzene) matrix was prepared by a radical suspension copolymerization. The matrix contained epoxy groups, so diethylaminohydroxypropyl groups were coupled to the matrix, leading to an anion-exchange resin. We studied the components, surface and pore structures of the anion-exchange resin by Fourier transform infared spectroscopy and scanning electron microscopy (SEM). SEM observations showed that the resin abounded in macropores as large as 3 to 8 microns both in the surface and the interior. The back-pressure of the column packed with the resin was modest even at a high flow-rate (60.2 cm/min). Then, bovine serum albumin (BSA) was used as a model protein to examine the adsorption properties of the anion-exchange resin. The results showed that under optimum conditions the resin had a capacity as high as 22.8 mg BSA/g wet resin, or 68.7 mg/g dry resin. The adsorbed protein could be desorbed by increasing the liquid phase ionic strength. Most importantly, the matrix had little nonspecific adsorption for BSA before introducing the ion-exchange groups.     

阴离子交换整体柱对蛋白质的分离与纯化

分别用乙二胺、二乙胺、三乙胺将自制的以甲基丙烯酸缩水甘油酯(GMA)为单体、乙二醇二甲基丙烯酸酯(EDMA)为交联剂的整体柱修饰为弱、强阴离子交换整体柱。考察了该整体柱的性能,选择出分离蛋白质(牛血清白蛋白、溶菌酶和谷胱甘肽)的最佳实验条件,并在最佳分离条件下考察了这些蛋白质在整体柱上的色谱行为和该整体柱对纤维素降解酶的分离纯化情况。实验结果表明,该整体柱性能良好,可以实现对纤维素降解酶的快速分离与纯化。同时,实验也证明采用梯度洗脱可以实现对某些蛋白质的分离纯化。     

强碱阴离子交换树脂及碱性洗脱剂的离子排阻/阴离子交换色谱法同时测定NH4+ ，NO2-和NO3-（英文）

Ion-exclusion/anion-exchange chromatography(IEC/AEC) on a combination of a strongly basic anion-exchange resin in the OH——form with basic eluent has been developed.The separation mechanism is based on the ion-exclusion/penetration effect for cations and the anion-exchange effect for anions to anion-exchange resin phase.This system is useful for simultaneous separation and determination of ammonium ion(NH+4),nitrite ion(NO-2),and nitrate ion(NO-3) in water samples.The resolution of analyte ions can be manipulated by changing the concentration of base in eluent on a polystyrene-divinylbenzene based strongly basic anion-exchange resin column.In this study,several separation columns,which consisted of different particle sizes,different functional groups and different anion-exchange capacities,were compared.As the results,the separation column with the smaller anion-exchange capacity(TSKgel Super IC-Anion) showed well-resolved separation of cations and anions.In the optimization of the basic eluent,lithium hydroxide(LiOH) was used as the eluent and the optimal concentration was concluded to be 2 mmol/L,considering the resolution of analyte ions and the whole retention times.In the optimal conditions,the relative standard deviations of the peak areas and the retention times of NH+4,NO-2,and NO-3 ranged 1.28%-3.57% and 0.54%-1.55%,respectively.The limits of detection at signal-to-noise of 3 were 4.10 μmol/L for NH+4,1.87 μmol/L for NO-2 and 2.83 μmol/L for NO-3.     

A chelate-forming resin bearing mercapto and azo groups and its application to the recovery of mercury(II)

A new chelate-forming resin bearing mercapto and azo groups was prepared from a common anion-exchange resin by treatment with azothiopyrine disulphonic acid (ATPS). ATPS resin was very stable and highly effective for the collection of mercury(II) by the batch and column methods. In the column method, the amount of mercury(II) in solution could be reduced to below 0.5 mug/l. The mercury(II) adsorbed could be eluted with thiourea solution, and the resin could be used repeatedly.     

离子排斥色谱结合光度检测的水质监测系统用于测定离子型营养物（英文）

A unified ion-exclusion chromatography(IEC) system for monitoring anionic and cationic nutrients like NH + 4,NO 2,NO 3,phosphate ion,silicate ion and HCO 3 was developed and applied to several environmental waters.The IEC system consisted of four IEC methodologies,including the IEC with ultraviolet(UV) detection at 210 nm for determining NH + 4 on anion-exchange separation column in OH form connected with anion-exchange UV-conversion column in I form in tandem,the IEC with UV-detection at 210 nm for determining simultaneously NO 2 and NO 3 on cation-exchange separation column in H + form,the IEC with UV-detection at 210 nm for determining HCO 3 on cation-exchange separation column in H + form connected with anion-exchange UV-conversion column in I form in tandem,and the IEC with visible-detection based on molybdenum-blue reaction for determining simultaneously silicate and phosphate ions on cation-exchange separation column in H + form.These IEC systems were combined through three manually-driven 6-port column selection valves to select each separation column to determine selectively the ionic nutrients.Using this sequential water quality monitoring system,the analytical performances such as calibration linearity,reproducibility,detection limit and recovery were also tested under the optimized chromatographic conditions.This novel water quality monitoring system has been applied successfully for the determination of the ionic eutrophication components in sub-urban river waters.     

Automated flow immunoassay for detection of food allergen using anion-exchange resin and alkaline phosphatase conjugated immunoglobulin G

A novel automated flow immunoassay system is developed for the detection of wheat protein as a food allergen. A polyclonal immunoglobulin G (IgG) antibody was isolated from serum of a rat with a wheat allergy, then reductively treated using dithiothreitol and covalently coupled to alkaline phosphatase. This conjugate was used in a non-competitive binding assay. The automated system was equipped with an immunoreaction column, an anion-exchange column, a luminescent reaction column and a photodetector. Antibody–antigen complexes were separated from their free conjugate on the basis of a difference in isoelectric point (pI) by an anion-exchange column. This simple technique permits the assay of wheat-protein allergen in 25 min with a reliable detection limit of 5 μg/ml. The anion-exchange column was regenerated by occasional elution with N-methylpiperazine buffer (pH 5.0) containing 0.5 M NaCl, to remove free conjugate. Free conjugate recovered in this manner could be reused up to four times without significant decrease in sensitivity of the immunoassay.     

Selectivity of monolithic supports under overloading conditions and their use for separation of human plasma and isolation of low abundance proteins

Human serum albumin (HSA) and immunoglobulin G (IgG) represent over 75% of all proteins present in human plasma. These two proteins frequently interfere with detection, determination and purification of low abundance proteins that can be potential biomarkers and biomarker candidates for various diseases. Some low abundance plasma proteins such as clotting factors and inhibitors are also important therapeutic agents. In this paper, the characterization of ion-exchange monolithic supports under overloading conditions was performed by use of sample displacement chromatography (SDC). If these supports were used for separation of human plasma, the composition of bound and eluted proteins in both anion- and cation-exchange mode is dependent on column loading. Under overloading conditions, the weakly bound proteins such as HSA in anion-exchange and IgG in cation-exchange mode are displaced by stronger binding proteins, and this phenomenon was not dependent on column size. Consequently, small monolithic columns with a column volume of 100 and 200 μL are ideal supports for high-throughput screening in order to develop new methods for separation of complex mixtures, and for sample preparation in proteomic technology.     

高效阴离子交换色谱-铜/铂修饰电极安培法测定大观霉素

采用阴离子交换色谱分离,在CuSO4溶液中加入少量镧系化合物,经电沉积制备La3+-Cu/pt/CME工作电极,建立了直流安培电化学法(DC)直接检测硫酸大观霉素的方法。考察了流动相浓度、测定电位等参数对色谱分离和测定的影响。在固定相为CarboPac PA10阴离子交换柱、流动相为26mmol/L NaOH,流速为0.6mL/min的色谱条件下,检测电位为0.68V时,硫酸大观霉素峰面积与其浓度在0.12～12mg/L(r=0.9991)和12～280mg/L(r=0.9995)两个范围内呈线性。本方法不需要柱前和柱后衍生化,能同时测定硫酸大观霉素中的主要组分和杂质。修饰电极制作方法简单,催化稳定性好,可作为电化学传感器测定硫酸大观霉素中的各组分。     

Improved recovery of trace amounts of gold (III), palladium (II) and platinum (IV) from large amounts of associated base metals using anion-exchange resins

The adsorption and desorption behaviors of gold (III), palladium (II) and platinum (IV) were surveyed in column chromatographic systems consisting of one of the conventional anion-exchange resins of large ion-exchange capacity and dilute thiourea solutions. The noble metals were strongly adsorbed on the anion-exchange resins from dilute hydrochloric acid, while most base metals did not show any marked adsorbability. These facts made it possible to separate the noble metals from a large quantity of base metals such as Ag (I), Al (III), Co (II), Cu (II), ¶Fe (III), Mn (II), Ni (II), Pb (II), and Zn (II). Although it used to be very difficult to desorb the noble metals from the resins used, the difficulty was easily overcome by use of dilute thiourea solutions as an eluant. In the present study, as little as 1.00 μg of the respective noble metals was quantitatively separated and recovered from as much as ca. 10 mg of a number of metals on a small column by elution with a small amount of dilute thiourea solution. The present systems should be applicable to the separation, concentration and recovery of traces of the noble metals from a number of base metals coexisting in a more extended range of amounts and ratios.     

Improved recovery of trace amounts of gold (III), palladium (II) and platinum (IV) from large amounts of associated base metals using anion-exchange resins

The adsorption and desorption behaviors of gold (III), palladium (II) and platinum (IV) were surveyed in column chromatographic systems consisting of one of the conventional anion-exchange resins of large ion-exchange capacity and dilute thiourea solutions. The noble metals were strongly adsorbed on the anion-exchange resins from dilute hydrochloric acid, while most base metals did not show any marked adsorbability. These facts made it possible to separate the noble metals from a large quantity of base metals such as Ag (I), Al (III), Co (II), Cu (II), Fe (III), Mn (II), Ni (II), Pb (II), and Zn (II). Although it used to be very difficult to desorb the noble metals from the resins used, the difficulty was easily overcome by use of dilute thiourea solutions as an eluant. In the present study, as little as 1.00 microg of the respective noble metals was quantitatively separated and recovered from as much as ca. 10 mg of a number of metals on a small column by elution with a small amount of dilute thiourea solution. The present systems should be applicable to the separation, concentration and recovery of traces of the noble metals from a number of base metals coexisting in a more extended range of amounts and ratios.