Study on the Separation of Co^(2+) from Zn^(2+) , Cd^(2+) by Anion-exchange Chromatography

The separation of Co 2+ from Zn 2+ , Cd 2+ by anion exchange chromatography was discussed. The chromatographic column containing anion resin 201×7 which was saturated with a solution of ammonium chloride. The effects of the eluant acidity and eluant composition on the separation were investigated. The results indicate that this anion exchange chromatography is suitable to the separation of Co 2+ from Zn 2+ , Cd 2+ , and the condition of separation is simple and convenient. When the column is saturated with NH 4Cl solution (2.0 mol/L, pH=4.0), the separation can be completed effectively. Zn 2+ and Cd 2+ can also be separa ted when different eluants are used and the pure solution with high concentration of Zn 2+ , Cd 2+ respectively can be obtained ea sily.

Determination of petroleum sulfonates in crude oil by column-switching anion-exchange chromatography

A column-switching anion-exchange chromatography method was described for the separation and determination of petroleum monosulfonates （PMS） and petroleum disulfonates （PDS） in crude oil that was simply diluted with the dichloromethane/methanol （60/40）. The high performance liquid chromatography （HPLC） system consisted of a clean-up column and an analytical column, which were connected with two six-port switching valves. Detection of petroleum sulfonates was available and repeatable. This method has been successfully applied to determine PMS and PDS in crude oil samples from Shengli oil field.

Copper modified platinum electrode for amperometric detection of spectinomycin sulfate by anion-exchange chromatography

A La^3＋-Cu/Pt modified electrode was fabricated by electrodepositing process in CuS04 solution by adding a small amount of lanthium compound, and it was employed for direct current （DC） amperometric detection of spectinomycin by anion-exchange chromatography. Without derivatization, this method can simultaneously determine the main component and impurities in spectinomycin pharmaceutical raw material. Ease of preparation, being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor for the determination of spectinomycin.

Refolding with Simultaneous Purification of Recombinant Human Granulocyte Colony-stimulating Factor from Escherichia coli Using Strong Anion Exchange Chromatography

The urea denatured recombinant human granulocyte colony-stimulating factor (rhG- CSF) which was expressed in Escheriachia coli (E. coli) was refolded with simultaneous purification by strong anion exchange chromatography (SAX) in the presence of low concentration- of urea. The effect of urea concentration on this refolding process was investigated. The obtained refolded rhG-CSF has a high specific activity of 2.3×108 U/mg, demonstrating that the proteins were completely refolded during the chromatographic process. With only one step by SAX in 40 min, purity and mass recovery of the refolded and purified rhG-CSF were 97% and 43%, respectively.

A novel composite stationary phase composed of polystyrene/divinybenzene beads and quaternized nanodiamond for anion exchange chromatography

An approach for preparation of a novel composite anion exchanger composed of polystyrene/divinylbenzene (PS/DVB) beads and quaternized nanodiamods (QND) were proposed. Oxidized nanodiamonds (OND) were quaternized by the condensation polymerization between methylamine (MA) and 1,4-butanediol diglycidyl ether (BDDE), which were characterized by Fourier transform infrared (FTIR) spectra, X-ray phtoelectron spectroscopy (XPS), thermogravimetric analysis (TGA). QND with layers of cationic polyelectrolyte was attached onto the surface of sulfonated PS/DVB beads electrostatically. Subsequently, hyperbranched reaction of QND agglomerated on the PS/DVB bead surface was performed by the alternate reaction between MA and BDDE to increase the exchange capacity. The composite anion exchanger showed good stability in organic solvent and a wide pH range.The surface of these microspheres was characterized by scanning electron microscopy. In addition, ion exchange selectivity and separation efficiency of the anion exchangers were assessed using the mixtures of anions (F,Cl,NO_2,Br,NO_3,HPO_4~2 and SO_4~2) with carbonate/bicarbonate as eluent, and the anion exchanger with high exchange capacity could be used to analyze chloride in aqueous solution with high concentration of fluoride. This work explores the potential of nanodiamods as an agglomerated material for ion chromatography stationary phases for the separation of inorganic anions.

Determination of zidovudine using anion exchange chromatography with integrated pulsed amperometric detection

A rapid and practical method for direct detection of zidovudine in high performance anion exchange chromatography （HPAEC） has been developed with integrated pulsed amperometric detection （IPAD）. Dionex AS18 （250mm × 2mm） and AG18 （50 mm× 2 mm） columns and 11 mmol/L NaOH solution were used for separation. Multi-step potential waveform parameters were optimized to maximize the signal-to-noise ratio （S/N）. Utilizing an optimized waveform, the repeatability （intra-day） precision and intermediate （inter-day） precision are obtained with relative standard deviation （RSD） of 1.88, 2.27, respectively. The limit of quantification （LOQ） and limit of detection （LOD） were found to be 9.70, 3.0 ng/mL, respectively, with correlation coefficients of 0.9992 over concentration range 0.01-10 μg/mL. The present method was successfully applied to the determination of zidovudine in human plasma. The recoveries of plasma sample spiked by 0.7 μg/mL, 2.7 μg/mL obtained were 95.3-101.5%, with relative standard deviation （RSD） of 2.54%, 2.21%, respectively.

Determination of lisinopril using anion exchange chromatography with integrated pulsed amperometric detection

A rapid and practical method for direct detection of lisinopril in anion exchange chromatography（AEC） has been developed with integrated pulsed amperometric detection（IPAD）.Dionex AS 18（250 mm×2 mm） and AG 18（50 mm×2 mm） columns and 40 mmol/L NaOH solution were used for separation.Multi-step potential waveform parameters were optimized to maximize the signal-to-noise ratio（S/N）.Utilizing the optimized waveform,the repeatability（intra-day） precision and intermediate（inter-day） precision were obtained with relative standard deviation（RSD） of 0.74,0.93,respectively.The limit of quantification（LOQ） and limit of detection（LOD） were found to be 0.37,0.12ng/mL,respectively,with the correlation coefficient of 0.9998 over concentration range 0.01-1μg/mL.The present method was successfully applied to the determination of lisinopril in human plasma.The recoveries of plasma sample spiked by 0.2μg/mL,0.8μg/mL lisinopril were 98.31-103.23%with RSD of 1.41%, 0.61%,respectively.

阴离子交换色谱法同时测定乳酸钠林格注射液中乳酸钠和总氯含量

目的建立同时测定乳酸钠林格注射液中乳酸钠和总氯含量的阴离子交换色谱法。方法分析柱为Dionex IonPac^(TM)AS11-HC柱(250 mm×4 mm),保护柱为AS11-HC柱(50 mm×4 mm),淋洗液为10 mmol/L氢氧化钾溶液,流速为1.0 mL/min,检测器温度为35℃,柱温为30℃,电导检测器,抑制器抑制电流为25 mA,进样量为25μL。结果乳酸根离子、氯离子质量浓度分别在9.97~249.37μg/mL、15.27~381.70μg/mL范围内与峰面积线性关系良好(r=0.9997,1.0000,n=6);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为100.74%,100.48%,RSD分别为1.17%,1.53%(n=9)。结论所建立的方法操作简便,灵敏度高,稳定性好,结果准确,可用于测定乳酸钠林格注射液中乳酸钠和总氯的含量。

饮用水中5种阴离子的离子色谱测定法

目的研究电导-离子色谱法同时测定水中5种阴离子的分析方法。方法用正交实验法L9(34)选择IC-2000型离子色谱仪的最佳实验条件,并在该条件下,将水样经0.45μm微孔滤膜过滤后直接利用离子色谱仪同时测定F-、Cl-、NO2-、SO42-、NO3-阴离子浓度。结果最佳流速和柱温分别为1.2ml/min和35℃,方法的RSD%均小于5.0%,各离子加标回收率为90%～106.7%,F-、Cl-、NO2-、SO42-、NO3-标准曲线回归方程的相关系数分别为0.9997,0.9999,0.9905,0.9999,0.9999。结论该方法具有准确、简便、快速、样品无须前处理等优点,可用于饮用水样品中5种阴离子的同时分析。

阴离子交换色谱中淋洗液流速对测定灵敏度影响的讨论

研究了阴离子交换色谱法定量分析时淋洗液流速对测定灵敏度影响的规律。使用３种不同型号的阴离子交换柱，详细地研究了３种总离子浓度不同的样品中淋洗液流速对峰高和峰面积的影响。实验表明，若标准溶液和样品溶液中的阴离子总浓度相差较大，将在不同程度上影响分析结果的准确度。初步探讨了上述现象的机理。通过紫外（２１０ｎｍ）和电导检测结果的对比观察，说明灵敏度的变化不完全如文献中提到的由抑制器抑制不足或ＮＯ－２质子化所致。在相同条件下改变柱温后的实验结果表明也不是离子交换过程中离子传质速度比较慢引起离子交换不完全的原因。提出的其它机理假设仍需进一步研究证实。

酪蛋白磷酸肽(CPPs)的纯化研究

研究了用大孔强碱性阴离子交换树脂提纯酪蛋白磷酸肽（ CPPs）的方法。结果表明，树脂 GM201对 CPPs的分离提纯效果较好，最佳洗脱纯化工艺条件为：盐酸浓度 0.2mol/L， NaCl浓度 0.3mol/L，温度 45℃。在上述最佳工艺条件下， CPPs回收率可达 77.7％～ 80％，纯度提高到 N:P=4.7:4.9。

蒙旦树脂化学组成的研究

采用阴离子交换色谱和硅胶－氧化铝柱色谱对云南寻甸蒙旦树脂（ＸＤＳＺ）、潦浒蒙旦树脂（ＬＨＳＺ）、昭通蒙旦树脂（ＺＴＳＺ）和吉林舒兰蒙旦树脂（ＳＬＳＺ）进行了族组分的分离。树脂游离酸，树脂结合酸，树脂烃和树脂醇在各树脂中的百分含量分别为ＸＤＳＺ１１．８６，８．７６，１２．３０，４５．９９；ＬＨＳＺ１５．８９，１３．９１，４．９０，４５．９９；ＳＬＳＺ２５．４６，８．０７，１７．４０，３６．２２；ＺＴＳＺ２Ｏ．００，１６．０９０３．８４，４５．５６。红外光谱结果表明，树脂是由分子量较小的正构酸、醇和烃以及具有上述官能团的环状，支链、芳构、饱和或不饱和以及特定结构内酯和其它含氧的各种化合物组成。单元化合物中存在着丰富的甲基，偕二甲基等。

阴阳离子交换色谱串联分离纯化苦瓜籽核糖体失活蛋白

将阴阳离子交换色谱柱在灌注色谱工作站上串联,使苦瓜籽粗提液中未被阴离子色谱柱吸附的蛋白质直接在阳离子色谱柱上吸附,用盐线性梯度洗脱从阳离子色谱柱上分离出两个具有抗真菌活性的蛋白。两个抗真菌蛋白经鉴定都达到了电泳纯,相对分子质量均为30000左右,N 端氨基酸序列分别为DVSFRLSGADPRSYGMFI与DVNFDLSTATAK,表明所得到的两种蛋白为苦瓜籽中的2个Ⅰ型核糖体失活蛋白α 苦瓜素(α MMC)和β 苦瓜素(β MMC)。抗菌实验表明,α MMC对香蕉枯萎菌和果腐霉菌均具有较强的抑制作用,β MMC对果腐霉菌有较强的抑制作用,而α MMC和β MMC对白绢菌的抑制活性均不明显。采用串联色谱,α MMC和β MMC的质量回收率分别为13 8%和8 0%。

高效阴离子交换-脉冲安培检测同时分析单糖和糖醛酸

建立了高效阴离子交换-脉冲安培检测（HPAE-PAD）同时分离测定8种单糖和2种糖醛酸的分析方法.以CarboPac PA20阴离子交换柱为分离柱,以2 mmol/L NaOH溶液将8种单糖从分离柱上洗脱,而后用NaAc（50～200 mmol/L）梯度淋洗2种糖醛酸,淋洗液流速为0.5 mL/min,总分析时间为30 min.在优化的分离测定条件下,8种单糖和2种糖醛酸的检出限为2.5～ 14.4 μg/L（进样体积25 μL,峰面积定量）.5 mg/L的10种化合物的混合标准溶液连续7次进样,峰面积的相对标准偏差为0.3%～ 1.5%.用所建立的方法测定了多糖水解液和木材半纤维素水解液中的单糖和糖醛酸含量.

高效阴离子交换色谱-电化学法测定酱油中的氨基酸

采用高效阴离子交换色谱-电化学检测器分离并测定了18种常见氨基酸. 实验首先对酱油样品进行了简单前处理, 然后以一定浓度的NaOH和NaAc溶液为淋洗液, 选择合适的梯度淋洗条件, 使18种氨基酸在阴离子交换色谱柱上实现良好地分离, 并用脉冲安培检测器进行了测定. 氨基酸的检出限为1.7～20.0 μg/L, 样品加标回收率在85%～108%范围内. 方法灵敏度高, 操作简单, 重现性好, 不需要繁琐的柱前或柱后衍生操作. 已应用到生抽和老抽酱油调味料产品中氨基酸的测定.

离子色谱法测定蓝藻培养液中有机酸和无机阴离子

建立了一种利用阴离子交换色谱柱分离,电导检测器同时测定17种有机酸和7种阴离子的方法。采用Ionpac AS11-HC阴离子交换柱,KOH溶液作为淋洗液,梯度洗脱,流量为1.0mL/min,柱温为30℃,进样体积为25μL。24种分析物测定结果的相对标准偏差在0.31%~2.67%之间,线性相关系数均大于0.996,平均加标回收率在80.3%~108.5%之间。该方法可用于微生物培养液中有机酸和阴离子的同时测定。

离子交换色谱测定原油中的单双石油磺酸盐

建立了一种新的离子交换高效液相色谱在线测定原油中单双石油磺酸盐的方法，通过使用六通阀切换，在一根强阴离子交换柱上完成在线纯化和分离。原油样品经过二氯甲烷-甲醇（体积比60：40）溶剂稀释后进入HPLC测定。原油中单石油磺酸盐的检出限为10．0μg/g，双石油磺酸盐的检出限为12．5μg/g。2-萘磺酸钠和萘-1，5-二磺酸钠分别在4.8～120．0mg／L和4．0～100．1mg／L范围内有良好的线性。该方法准确、重复性好，可以满足原油中石油磺酸盐的分离测定。

高效阴离子交换色谱分离-脉冲安培检测法测定烟草料液中的糖、糖醇和醇类化合物

建立了高效阴离子交换色谱分离-脉冲安培检测法测定烟草料液中的糖、糖醇以及醇类化合物的方法。以NaOH为淋洗液，在CarboPac MA1阴离子交换柱上等度分离了肌醇、甘油、丙二醇、半乳糖醇、木糖醇、山梨醇、甘露醇、葡萄糖、果糖、蔗糖、甘露糖和半乳糖等12种化合物。对影响分离和检测的条件进行了优化，并在此优化条件下分析了烟草料液中的糖、糖醇以及醇类化合物。12种化合物的检出限为2．0～216μg／L（25．0μL进样，以3倍信噪比计算检出限）。12种化合物浓度为1～5mg／L的标准溶液连续7次进样的RSD为0．7％～4．3％。方法对烟草料液中12种化合物的加标回收率为80％～108％。方法灵敏、高效、简便、快捷。

糖的高效阴离子交换色谱-脉冲安培检测法分析

高效阴离子交换色谱-脉冲安培检测法是新近发展的一种分析糖的有效方法。本文讨论了糖的高效阴离子交换色谱分离和脉冲安培法检测的原理,色谱条件的选择,包括分离糖的固定相、流动相以及检测糖的脉冲电位波形,并对方法的应用进行了较为详细的叙述。

阴离子交换色谱-积分脉冲安培检测法分离测定氨基酸注射液中的氨基酸和葡萄糖

用阴离子交换色谱 积分脉冲安培检测法测定了氨基酸注射液中 1 7种氨基酸和葡萄糖。研究了氨基酸和葡萄糖在阴离子交换色谱中的保留行为。采用了优化的水、NaOH和NaAc三元梯度淋洗条件。在优化的梯度淋洗条件和积分脉冲安培检测条件下 ,氨基酸和葡萄糖的检出限为 0 3pmol～ 1 0 3pmol,线性范围约为 2个数量级。样品加标回收率为 88 3 %～ 1 0 4 6 %。方法简单、灵敏。