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.

Imidazolium group prompted alkaline anion-exchange membrane with high performance for efficient electrochemical CO_(2) conversion

Development of high-performance hydroxide-conductive membranes is a focus research subject owing to promising applications in electrochemical reduction of CO_(2)(eCO_(2)RR).However,few satisfactory membranes have been developed to maximize the performance of CO_(2) electrolyzers,despite its role as the core in regulating ion transport and preventing product crossover or fuel loss.Herein,we report the synthesis of alkaline anion-exchange membranes fabricated by poly(vinyl-alcohol)(PVA)and poly[(3-methyl-1-vinylimidazoliummethylsulfate)-co-(1-vinylpyrrolidone)](PQ44)for use in CO_(2) electrolysis.Owing to the unique imidazolium ring structure coupled with a three-dimensional semiinterpenetrating porous internal architecture,the PVA/PQ44-OH-membranes provide a high hydroxide conductivity(21.47 mS cm^(-1)),preferable mechanical property and thermal stability.In particular,the eCO_(2)RR used PVA/PQ44-OH^(-) as electrolyte membrane realized a charming Faradaic efficiency(88%)and partial current density(29 mA cm^(-2))at0.96 VRHE and,delivered the excellent durability over 20 h electrolysis in 0.5 mol L^(-1) KHCO_(3) electrolyte.Notably,it can even enable an ultrahigh current density beyond 100 mA cm^(-2) at^(-1).11 VRHE when the electrolyte was KOH instead,and produced the FEHCOOof 85%at a low potential of0.81 VRHE,superior to both commercial alkaline A201 and acidic Nafion117 membrane.

Synthesis and characterization of quaternized poly(phthalazinone ether sulfone ketone)for anion-exchange membrane

Chloromethylated poly（phthalazinone ether sulfone ketone） （CMPPESK） was prepared from poly（phthalazinone ether sulfone ketone） （PPESK） using chloromethyl octyl ethers （CMOE） with lower toxicity as chloromethylated regent. CMPPESK was soluble in N-methyl-2-pyrrolidone （NMP）, N,N-dimethylacetamide （DMAc） and chloroform. Quaternized poly（phthalazinone ether sulfone ketone） （QAPPESK） was prepared from CMPPESK by quaternization. QAPPESK had excellent solvent resistance, which was only partly soluble in sulfuric acid （98%） and swollen in N,N-dimethylformamide （DMF）. The vanadium redox flow battery （V-RFB） using QAPPESK anion-exchange membrane had better performance with 88.3% of overall energy efficiency.

Phosphate removal from aqueous solution by Donnan dialysis with anion-exchange membrane

The removal of phosphate from aqueous solution by Donnan dialysis with anion-exchange membrane was investigated.The results show that phosphate could be removed from aqueous solution without supplying external high pressure or electrical potential.Under the conditions of influent phosphate of 2.0 mg/L,counterion(Cl-)concentration of 0.1 mol/L,stirring speed of 500 r/min and phase temperature of 298 K,the removal of phosphate achieves 70.0%.Decreasing counterion concentration has little influence on the removal of phosphate,but phosphate amount in anion-exchange membrane increases significantly.With the increase of stirring speed and phase temperature,the removal efficiency of phosphate greatly is improved.Existing forms of phosphate in aqueous solution affected transport of phosphate and only strong acidic pH of feed solution(pH=3.0)decreases the removal of phosphate.Transport of phosphate is also accompanied by change of pH value of feed solution.In consequence,it might be a promise potential process for phosphate advanced wastewater treatment,especially in the area where high salted nature water can be utilized.

Investigation on the Use of the Weakly Basic Polyacrylate Anion-Exchanger Amberlite IRA-68 for Sorption and Separation of Iminodiacetate Complexes of Rare Earth Elements

Based on the determined affinity series of rare earth element complexes with IMDA for the anion-exchangers, purification of macroquantities of Nd 3+ from Y 3+, Sm 3+ from Ho 3+, La 3+ from Nd 3+ and La 3+ from Pr 3+ on the weakly basic gel anion-exchanger Amberlite IRA-68 was studied. Using the presented method on 1 L of Amberlite IRA-68 in the acetate form, it is possible to obtain about 240 g Nd 2O 3 purified from Y 2O 3. Great difference in affinity of La 3+ and Nd 3+ as well as Pr 3+ complexes for this anion-exchanger in the acetate form indicates the possibility of applying this process for purification of lanthanum on the increased scale. On 1 L of Amberilte IRA-68 in the acetate form it is possible to obtain about 1125 g La 2O 3 purified from Nd 2O 3. On the basis of these results it can be assumed that unique properties of polyacrylate anion-exchangers enable their application for separation of rare earth elements.

Quantitation of metallothionein and cadmium in metallothionein in mink livers by anion-exchange HPLC-GFAAS method

Metallothionein (MT) has a great capacity of binding heavy metals showing an interesting connection with metal toxicology, as a biochemical marker for environmental metal pollution. Anino-exchange high per formance liquid chromatography (HPLC) was used to isolate and quantitate MT in livers of minks which were contaminated with heavy metals. MT isoforms (MT-I and MT-II) were eluted at approximately 11.3 and 14.3 min respectively from a DEAE-5 PW anion-exchange column with a Tris-HCl buffer (0.01 -0.25 mol/L, pH 8.6) and detected by UV absorbance at 254 nm. The cadmium concentrations in mink liver MT elutkms were determined by graphite furnace atomic absorption spectrometry (GFAAS) . Obvious increase in liver MT-I concentration rather than liver MT-II was found when the minks were contaminated by feeding contaminated fish captured from the heavy metal-polluted river. The cadmium concentration in mink liver MT-I also increased to some extent as the contaminated level increased.

Optimization of a Method for the Simultaneous Determination of Phloroglucinol and Trimethylphloroglucinol by High Performance Liquid Chromatography in Routine Use in a Pharmaceutical Industry in Abidjan

In order to provide the population with safe, effective and good quality medicines, the pharmaceutical industries, before releasing batches of their products into the pharmaceutical circuit, put in place internal dosage methods to control the quality of these products. The present study consisted in optimizing a method for the simultaneous determination of Phloroglucinol (PHG) and Trimethylphloroglucinol (TPH) by high performance liquid chromatography (HPLC) routinely used in a pharmaceutical industry located in a township in Abidjan (Ivory Coast). The basic chromatographic conditions were those routinely used for the determination of these two molecules: mobile phase: acetonitrile/water (60/40), stationary phase (C18 BDS Hypersil 250 mm * 4.6 mm - 5 μm), detection wavelength (265 nm), flow rate, injection volume and run time configured at the equipment level were respectively 1 mL/min, 10 μL and 8 min. The method of preparation of the analytes (PHG and TPHG) was also applied by the pharmaceutical industry. The application of these different parameters at the equipment level made it possible to determine a chromatogram which highlights three chromatographic peaks with respective retention times (RT) of 0.773 min (unidentified compound), 2.275 min (PHG) and 7.269 min for an analysis time of 8 min with a better resolution of the peaks and baseline. The progressive optimization of different parameters such as the stationary phase (C18 YMC 150 mm * 4.6 mm - 3 μm), the proportion of the mobile phase: acetonitrile/water (80/20), the flow rate impelled by the pump (0.8 mL/min) and the modification of the analyte preparation mode (same amount of PHG and TPHG in a 50 mL volumetric flask) resulted in a final chromatogram that highlighted two chromatographic peaks at the respective RT of 2.391 min (PHG) and 3.735 min (TPHG) at a run time of 6 min. The chromatographic conditions that led to the final chromatogram can be used routinely by the pharmaceutical industry for the determination of several PHG and TPHG drug matrices after prior validation of the determination method.

离子色谱指纹图谱分析在烟用香精香料品质评价中的应用

为保证烟用香精香料品质的一致性,采用离子色谱法对烟用香精香料样品中的9种有机酸及7种无机阴离子进行分析。1.0 g样品中加入10 mL去离子水,振荡萃取30 min后,水相溶液用0.45μm微孔滤膜过滤,滤液进一步采用RP前处理柱除去基质,经离子色谱仪分离测定。采用Dionex IonPac AS11-HC阴离子交换柱及淋洗液梯度洗脱,9种有机酸和7种常规无机阴离子标准工作溶液的保留时间和峰面积日内精密度(RSD)分别为0.01%~0.69%和1.34%~2.98%,日间RSD分别为0.03%~0.68%和3.54%~5.16%。同时对烟用香精香料标准样品A~D(各5个批次)中有机酸和无机酸的保留时间和峰面积RSD进行考察,得到的保留时间和峰面积日内RSD分别为0.01%~0.71%和2.39%~3.22%,日间RSD分别0.05%~0.81%和3.61%~6.02%。建立了4种烟用香精香料(各5个批次)的指纹谱图库,并采用系统聚类分析和相似度分析法对其他生产厂家样品进行品质评价。结果表明,聚类分析法能有效地从不同生产厂家的产品中筛选出与标准样品质量最相近的样品;实际样品AY3、BY2、CY2及DY1与香精香料标准品性质最接近,品质较好。相似度分析可以对不同生产厂家的产品质量进行更加具体、量化的评价,实际样品AY3、BY2、CY2及DY1与香精香料标准品的化学成分相似度值均大于97.7%,符合相似度评价要求。相较于超声辅助液液萃取-气相色谱法,对于个别特殊样品,离子色谱法能更有效地区分香精香料样品间的品质差异。

基于代谢组学对“英红9号”及其黄化突变种“黄玉”的红茶生产适制性比较分析

目的 探究“英红9号”黄化突变种“黄玉”的生产适制性。方法 通过广泛靶向的代谢组学和气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)分析了“英红9号”和“黄玉”鲜叶和发酵叶中主要代谢产物的差异,并测定二者间表观物质生化含量如叶绿素类胡萝卜素等,综合代谢物含量进行统计分析。结果 “黄玉”鲜叶中总叶绿素与类胡萝卜素的差值小于“英红9号”。“英红9号”中山奈酚-3-糖苷的含量更高,而“黄玉”中山奈酚-3-葡萄糖苷与山奈酚-3-O-半乳糖苷的比值更高。与“英红9号”鲜叶相比,“黄玉”中作为β-胡萝卜素必要前体物质的玉米黄质和棕榈酸玉米黄质的含量显著较高。“黄玉”发酵叶中由于类胡萝卜素降解能够产生花果风味的物质如:α-法内烯、β-环柠檬醛、橙花叔醇和反式香叶基丙酮的含量均高于“英红9号”。结论 “黄玉”鲜叶中β-葡萄糖苷酶和类胡萝卜素裂解双加氧酶的活性较高。这些代谢特征说明“黄玉”适合生产绿茶、白茶等发酵程度较低的茶。其高活性的酶有助于绿茶的香气和口感形成。相比之下,“英红9号”中的代谢物使其在发酵过程中产生更多的香气成分,如橙油醇和香叶酰丙酮的增加,表明它适合生产红茶。

胶黏剂产品中VOCs含量与类别的检测方法

可靠、高效的检测方法,能够准确测定胶黏剂产品中挥发性有机化合物(VOCs)的含量及类别,进而为胶黏剂产品生产提供参考,不断提升胶黏剂产品的环保安全性。一般采用气相色谱法、气相色谱-检测器联用法、气相色谱-质谱法,通过优化顶空条件、色谱柱选择和质谱参数,实现对目标VOCs的高灵敏度、高选择性检测。这些方法能够有效分离和定量分析胶黏剂产品中的多种VOCs,包括烷烃、烯烃、芳香烃、醛类、酮类等,获得了VOCs含量和类别分布的详细数据,为胶黏剂产品中VOCs含量和类别的检测提供了一种可靠、高效的解决方案,可用于评估胶黏剂产品的环境友好性,并为制定相关标准和法规提供技术支持。

纳米晶纤维素组装的手性介孔材料及其对手性药物的分离

纤维素纳米晶体(CNC)是由硫酸催化的纤维素水解制备的,根据纤维素的来源和水解条件,纳米晶体的直径约为5~15 nm,长度约为100~300 nm。CNC在水中可以形成具有手性向列型结构的液晶相。当干燥成固体薄膜时,CNC保持螺旋手性向列顺序并组装成层状结构。在CNC自组装过程中,可以添加溶胶-凝胶前体,如Si(OMe)_(4)。随着溶剂的蒸发,这些前体会发生水解和缩合,从而形成手性向列相二氧化硅/CNC复合材料。复合材料在空气中煅烧破坏纤维素模板,留下高表面积手性向列结构的介孔二氧化硅膜。此外,有机二氧化硅或二氧化钛薄膜也采用类似的方法得到。这些薄膜可用作滤光片、反射器和薄膜。最重要的是,合成的手性介孔二氧化硅可用作手性色谱固定相材料分离手性药物。结果显示,手性分离的效果显著,为CNC开发手性新材料提供了新方法。

高等农业院校现代色谱分析课程思政探索与实践

课程思政建设是当前加强高校思想政治工作和专业课程教学改革的重要内容,是构建全方位育人格局,将其他课程与思政课同向同行,协同育人,以最终实现“立德树人”根本教育任务的一种综合教育理念。现代色谱分析是高等农业院校化学、农学、食品科学、动物药学、动物医学等专业研究生的必修课程。该课程开课专业广、修读人数多,是开展课程思政教育的重要载体。作者以高等农业院校现代色谱分析课程为例,介绍了实施课程思政的重要意义,课程思政元素的挖掘及思政内容与专业内容的融合,希望能为相关学科课程思政教学提供有益参考。

液液萃取-气相色谱质谱法测定水质中的环氧氯丙烷

比较了不同前处理方法进行水质中环氧氯丙烷的测试,其中液液萃取的前处理方法简单可靠,方便易行,适合复杂基质水样的测定。同时比较了气相色谱仪不同检测器对环氧氯丙烷(ECH)的响应值,其中质谱检测器对ECH的响应值最高。液液萃取-气相色谱质谱法测定水质中的环氧氯丙烷,该方法的检出限为0.6μg/L,测定下限为2.4μg/L。对海水、地表水、工业污水样品加标浓度为0.001 mg/L、0.02 mg/L、0.2 mg/L进行平行6次测定,结果的相对标准偏差分别为6.9%、2.7%和6.3%,加标回收率分别为93.5%、99.0%和99.6%,非常适合各类水质ECH的监测。

不同干燥方式八角果实挥发性化合物代谢组分析

【目的】探明不同干燥方式对八角果实挥发性成分的影响,筛选出适宜八角果实干燥的处理方式,为八角后期深加工、保存及应用提供参考。【方法】以新鲜八角果实为材料,采用自然晾晒、40℃、50℃、60℃、70℃、80℃和90℃烘干7种处理方式进行干燥,通过液相色谱-质谱(LC-MS)技术检测分析八角果实代谢产物,阐明八角果实不同温度干燥与自然晾晒处理的代谢物差异。【结果】与自然晾晒相比,八角果实40℃干燥差异代谢产物有11类17种,其中,萜类、醇类和醛类3类代谢物上调;50℃干燥差异代谢物有10类25种,其中,上调代谢物6类(萜类、醇类、酯类、酮类、卤代烃类、酚类);60℃干燥差异代谢物有8类13种,其中,醇类和烃类代谢物上调;70℃干燥差异代谢物为13类40种,其中,醇类、萜类和酯类3类代谢物上调;80℃干燥差异代谢物有13类38种,仅醇类代谢物上调;90℃干燥差异代谢物有13类52种,其中,上调代谢物4类(萜类、醇类、酮类、卤代烃类)。40℃、50℃和60℃干燥的八角果实与自然晾晒差异代谢物较少,上调代谢物主要是苯甲醛、醋酸植物醇、茴香脑、6-异羟基樟脑、乙酸异丁香酚酯和甲基丁香酚等挥发性化合物,提升了八角浓厚的香味。70℃、80℃和90℃干燥的八角果实与自然晾晒差异代谢物较多,且与八角香味相关的许多代谢物下调表达,主要有香芹酮、茴香脑、E-氧化玫瑰、4-蒈烯、对薄荷脑1,5,8-三烯、苯甲醛、芳樟醇、3-甲基苯并噻吩、2-甲基-2-四氢呋喃和2-乙酰基-5-甲基呋喃等挥发性化合物,减弱了八角香味。【结论】不同干燥处理八角果实的挥发性化合物种类均存在一定差异。40℃、50℃和60℃干燥八角果实,苯甲醛、醋酸植物醇和茴香脑等上调表达的挥发性化合物提升了八角香味。八角果实经50℃干燥后,上调表达的代谢物有萜类、醇类、酯类、酮类、卤代烃类和酚类6类,果实独特香气保持最好,宜在生产上推广应用。

固相萃取-超高效液相色谱-三重四极杆/线性离子阱质谱法检测水中大环内酯类抗生素

采用固相萃取-超高效液相色谱-三重四极杆线性离子阱质谱技术(SPE-UPLC-QTRAP MS)建立了环境水样中阿奇霉素、林可霉素、克林霉素、红霉素及替米考星5种大环内酯类抗生素的检测方法。调节水样pH为10后经HLB固相萃取柱净化、富集,然后用Kinetex F5色谱柱进行分离,用0.1%甲酸水溶液和0.1%甲酸乙腈溶液进行洗脱,采用电喷雾正离子源(ESI+),多反应监测(MRM)-信息依赖采集(IDA)-增强子离子(EPI)扫描模式对样品进行检测,用多反应监测(MRM)进行定量,增强子离子(EPI)谱图库辅助定性。结果表明:5种大环内酯类抗生素线性关系良好,相关系数均大于0.9992;检出限为0.01~0.30μg·L^(-1),定量限为0.10~0.50μg·L^(-1);3种不同浓度的水样加标回收率为71.60%~111.05%,相对标准偏差均在10%以内,EPI谱库比对纯度值均大于90%。该方法将传统的MRM扫描模式结合EPI谱图库检索,实现了同时定性和定量分析,对未知物准确定性定量检测提供了重要参考。

色谱技术在纺织服装化学残留物检测中的应用

纺织服装生产过程中使用的各种染料、助剂等会形成化学残留物,不仅会对人体健康产生风险,也会影响生态系统的健康发展。色谱技术具有高分离效率和准确的定量能力等优势,可以有效检测纺织服装中的化学残留物,有利于保护消费者健康,减少环境污染。探讨色谱技术在纺织服装化学残留物检测中的应用,可以为纺织行业提供理论参考。

科研成果转化为教学资源对提升教学效果的作用:以药物分析学课程中色谱方法的教学为例

药物分析学课程是将多个课程联系起来形成新的综合知识节点的三维知识网,涉及知识体系庞大,知识结构灵活。其中,色谱分析法在这门课程中涉及面极广,要准确掌握其内容难度很大,这会导致教学效果不好。本着立德树人的教育宗旨和培养复合型高素质专业人才的目标,本文以药物分析学课程中色谱方法的教学为例,将与色谱方法相关的科研成果转化为教学资源,融入教学过程,将创新理念和科研思路渗透给学生,这不仅有利于学生理解并掌握知识,而且能够锻炼学生提出问题和解决问题的能力。本文进一步阐述了如何通过课程设计引入科学发展前沿并渗透科学问题,从而阐明将科研成果转化为教学资源对达成教学目标的促进作用。针对药物分析学课程知识更新速度快、理论与实践并重的特点,我们通过引入色谱科学发展前沿、渗透科学问题、采用问题式与任务驱动式相结合的教学方法对课程进行设计,并采用多元化考核、学生反馈、自我评价3个方面对教学效果进行评估。结果表明,将科研成果转化为教学资源对激发学生学习兴趣、提升学生解决问题的能力,以及达成课程目标具有显著作用,在很大程度上提升了教学效果,实现了学生知识、能力和素质的共同提高。

QuEChERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定蜂房及其制剂中10种真菌毒素

目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测(MRM)模式下进行测定,内标法定量。结果 10种真菌毒素含量在各自质量浓度范围内具有较好的线性关系(r>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为83.8%~107.1%(RSD<6.5%),定量限(LOQ)为0.18~129μg/kg。结论 该法前处理步骤简便,净化效果良好,提高了样品检测效率,内标法定量精准可靠,适用于蜂房及其制剂中10种真菌毒素的同时检测。

采用自主研发的在线前处理系统同时分析脱硫废水中阴阳离子

电厂专用的全自动脱硫废水分析仪可以实现对超高浓度脱硫废水的自动化前处理以及分析,样品通过自动二步稀释,并与双系统离子色谱仪联用,对脱硫废水中的阴、阳离子同时进行检测。脱硫废水中阳离子主要有Na+、NH4+、K+、Mg2+、Ca2+,阴离子主要有F-、Cl-、NO3-、SO42-。本研究对仪器相关参数进行了验证,测试结果为,4种阴离子和5种阳离子的混合标准溶液在其线性关系内相关系数均大于0.999;4种阴离子的峰高和峰面积重复性RSD小于2.29%,5种阳离子的峰高和峰面积重复性RSD小于1.78%,实际样品中4种加标阴离子回收率在93.5%~100.2%之间;5种阳离子加标回收率在95.4%~103.8%之间。结果证明,该系统大大提高了分析效率,节省了人工成本,填补了市场空白。