离子排斥色谱法测定黄酒中的13种有机酸

建立了离子排斥色谱法（ ion-exclusion chromatography，IEC）测定黄酒中有机酸含量的分析方法。使用Waters 离子排斥色谱柱（300 mm×7.8 mm，7μm），流动相为 H 2 SO 4溶液（ A）与乙腈（ B）的混合溶液（体积比为98：2），线性梯度程序：0～40 min，流动相 A 的浓度由0.01 mol / L 上升到0.02 mol / L；40～50 min，流动相 A 的浓度为0.01 mol / L ；流速为0.5 mL / min，柱温50℃，进样量10μL，检测波长210 nm。结果表明，该方法可在30 min内实现草酸、马来酸、柠檬酸、酒石酸、苹果酸、抗坏血酸、琥珀酸、乳酸、富马酸、乙酸、丙酸、异丁酸和丁酸的完全分离与定量，13种有机酸在0.001～1.000 g / L 范围内线性关系良好，回归方程的线性相关系数在0.9997以上。黄酒中13种有机酸的加标回收率为93.4％～103.8％，相对标准偏差为0.1％～1.5％（n =5）。该方法简单快捷、准确、重复性好，可用于黄酒中有机酸的测定。

直接电导检测离子排斥色谱法测定C_1～C_6脂肪族有机酸

建立了直接电导检测离子排斥色谱分离测定C1-C6脂肪族有机酸（甲酸、乙酸、丙酸、丁酸、戊酸、己酸）的方法。以Shim-pack SCR-102H色谱柱为分离柱,选用p-甲苯磺酸水溶液为流动相,考察了流动相中p-甲苯磺酸的浓度、流速、pH、色谱柱温度对分离和测定脂肪族有机酸的影响,确定了最佳的色谱条件为：0.2mmol/Lp-甲苯磺酸水溶液作为流动相,流速1.2mL/min,柱温45℃。所测有机酸的检测限为0.03-0.99mg/L,相对标准偏差在2.3%以下（n=5）,回收率为91.2%-105.6%,整个分析过程在28min内完成。该法用于白酒样品的分析,结果令人满意。

直接电导检测-离子排斥色谱法测定碳酸氢根

发展了直接电导检测一离子排斥色谱测定碳酸氢根的方法。以Shim-pack SCR-102H离子排斥色谱柱为分离柱,选用对羟基苯甲酸为淋洗液。考察了淋洗液浓度、流速、色谱柱温度对碳酸氢根保留时间的影响。确定最佳色谱条件为:以0.1 mmol/L对羟基苯甲酸为淋洗液,流速1.0 mL/min,色谱柱温度40℃。在此条件下,碳酸氢根的保留时间在12 min之内,检出限(SIN=3)为0.8 mg/L,连续5次测定峰面积的相对标准偏差为0.4%。将方法应用于可乐样品的分析,加标回收率为96.5%。

Determination of Uric Acid in Human Urine by Ion-exclusion Chromatography with UV Detection Using Pure Water as Mobile Phase

A simple, rapid and accurate ion-exclusion chromatographic method coupled with a UV detector for the determination of uric acid in human urine samples has been developed. The separation was carried out on an ion-exclusion column using only pure water as mobile phase. The detection wavelength was 254 nm and urine sample was injected directly without any pretreatment. Furthermore, the retention behavior of uric acid on the ion-exclusion column was researched when pure water and 1 mmol·L-1 HCI were used as mobile phase, respectively. The stability of uric acid was also further investigated within 28 days, In this method, the linear range of the calibration curve for uric acid was 0.25--100 mg·L-1, and the detection limit calculated at S/N=3 was 0.02mg·L-1 The proposed ion-exclusion chromatographic method has been used for the determination of uric acid in human urine.

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.

Microcomputer Simulation of Elution Behaviour for Dicarboxylic Acids in Ion－Exclusion Chromatography

he present paper covers a model involving Donnan memhrane equilibrium andadsorption eluilibrium to describe the retention process for diprotic organic acids inion-exclusion chromatography. On this basis the microcomputer simulation of elu-tion behaviour for dicarboxylic acids was investigated. Influences of eluent acidityand sample concentration on the retention value were studied. The theoreticallypredicted results are in reasonable agreement with the experimental data.

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NH_4^+，NO_2^-和NO_3^-(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.

离子排斥色谱用于厌氧消化处理的水中脂肪族羧酸的分析(英文)

The analysis of seven aliphatic carboxylic acids(formic,acetic,propionic,iso-butyric,n-butyric,iso-valeric and n-valeric acid) in anaerobic digestion process waters for biogas production was examined by ion-exclusion chromatography with dilute acidic eluents(benzoic acid,perfluorobutyric acid(PFBA) and sulfuric acid) and non-suppressed conductivity/ultraviolet(UV) detection.The columns used were a styrene/divinylbenzene-based strongly acidic cation-exchange resin column(TSKgel SCX) and a polymethacrylate-based weakly acidic cation-exchange resin column(TSKgel Super IC-A/C).Good separation was performed on the TSKgel SCX in shorter retention times.For the TSKgel Super IC-A/C,peak shape of the acids was sharp and symmetrical in spite of longer retention times.In addition,the mutual separation of the acids was good except for iso-and n-butyric acids.The better separation and good detection was achieved by using the two columns(TSKgel SCX and TSKgel Super IC-A/C connected in series),lower concentrations of PFBA and sulfuric acid as eluents,non-suppressed conductivity detection and UV detection at 210 nm.This analysis was applied to anaerobic digestion process waters.The chromatograms with conductivity detection were relatively simpler compared with those of UV detection.The use of two columns with different selectivities for the aliphatic carboxylic acids and the two detection modes was effective for the determination and identification of the analytes in anaerobic digestion process waters containing complex matrices.