Determination of uric acid in human urine by ion chromatography with conductivity detector

A simple,fast,precise and eco-friendly analytical method for the determination of uric acid(UA) in human urine by ion chromatography(IC) was established.The sample pretreatment was not required,only needed centrifugation and filtration.The separation was carried out on a cation exchange column with 2.0 mmol/L nitric acid as mobile phase at the flow-rate 1.0 mL/min.A non-suppressed conductivity detector was used.The IC analysis time for one run was within 10 min under the optimized IC condition.The detection limits were 0.5μg/L(S/N = 3) for uric acid.The recovery was 100.1%while the relative standard deviation (RSD) was 1.8%from 10 measurements.     

Determination of paracetamol in dosage forms by non-suppressed ion chromatography

An ion-chromatography procedure for the simultaneous determination of paracetamol and salicylic acid without suppression using UV detection is proposed. The method is applied to the determination of paracetamol in pharmaceuticals and also permits the quantitation of the total acetylsalicylic acid as salicylic acid.     

Determination of benzoic acid in milk by solid-phase extraction and ion chromatography with conductivity detection

A simple, fast, precise and eco-friendly method, based on ion chromatography (IC) with a suppressed conductivity detector, was proposed for the determination of benzoic acid (BA) inmilk in this paper. The chromatographic separation was accomplished by using an anion exchange column eluted with 3.2 μmol/L aqueous Na2CO3 and 1.0 mmol/L aqueous NaHCO3 at a flow-rate of 0.7 mL/min. Themethod validation experiment provided excellent results with respect to linearity (correlation coefficient up to 0.9997), limit of detection (0.1 μg/L), recovery values (ranging from 88.0% to 93.0%) and relative standard deviation (RSD) (below 2.2%, n = 7).     

食品中亚硫酸盐的离子色谱法测定

建立了食品中亚硫酸盐的离子色谱检测方法. 样品采用40 mmol/L NaOH溶液提取, 甲醛作稳定剂, 经ENVI-Carb活性碳小柱除去提取液中的色素, 石油醚除去提取液中的油脂, 用配有电导检测器的离子色谱仪测定. 以AS9-HC为色谱柱, 流动相为8 mmol/L Na2CO3-2.5 mmol/L NaOH, 亚硫酸盐的残留量在0～6.0 mg/L的范围内线性关系良好, 相关系数为0.9989, 相对标准偏差为1.3%～9.1%, 回收率在88.4%～98.1%之间.     

离子色谱法测定土壤中植物激素乙烯利

土壤样品中的乙烯利在IonPac AS14分离柱（4mm）,（3．5mmol Na2CO3＋1．0mmol NaHCO3）／L淋洗液的淋洗条件下得到较好的分离。在0～10μg／mL的范围内标准曲线呈线性,检出限为（0．08μg／mL）。精密度好,10．266μg／mL时,保留时间的RSD=0．86％;峰高的RSD=1．1％;峰面积的RSD=1．0％。在此条件下,其它阴离子对乙烯利的检测不干扰,样品的加标回收率为85．6％～87．9％。     

柱前衍生高效液相色谱法测定二乙醇胺脱氢产物亚氨基二乙酸和甘氨酸

以对甲苯磺酰氯(PTSC)为衍生剂,建立了柱前衍生高效液相色谱(HPLC)测定二乙醇胺脱氢产物中亚氨基二乙酸(IDA)和甘氨酸(Gly)含量的分析方法。IDA和Gly与衍生剂在碱性(pH 11)条件下于45℃反应15 min,进行柱前衍生,并利用高效液相色谱-质谱对衍生产物进行定性分析。衍生化产物采用VP-ODS色谱柱(200 mm×4.6 mm,5μm)分离,以0.03 mol/L醋酸铵溶液(pH 5.5)为流动相A、乙腈为流动相B(体积比为87∶13),进行等度洗脱,流速为1 mL/min,并采用配有紫外检测器的高效液相色谱仪测定,检测波长为235 nm。该法在IDA质量浓度为900~2 100 mg/L、Gly质量浓度为20~100 mg/L的范围内线性关系良好,相关系数(R2)均大于0.999。IDA和Gly的检出限(LOD)分别为0.089 7 mg/L和0.026 2 mg/L,加标回收率分别为98.7%~99.3%和98.0%~99.5%,相对标准偏差(RSD)分别为0.89%~1.23%和0.95%~1.11%(n=3)。该法具有反应条件温和、准确性高的特点,可用于工艺生产中IDA和Gly含量的测定。     

离子色谱法测定乙二醇中微量有机酸和无机阴离子

建立了以YSA-8阴离子交换柱的离子色谱法分析乙二醇中微量有机酸和无机阴离子的方法,比较了进样乙二醇浓度对F-及有机酸测定结果的影响,进样乙二醇质量分数低于8.5%时,能够得到较准确的数据.用本法对所测的有机酸和无机阴离子检出限均在8.9 μg/L以下,线性相关系数r在0.996～0.999范围内,标准样中各物质的离子峰面积的相对标准偏差(RSD)在4.2%以下(n＝11),对乙二醇质量分数约为8.5%的样品中F-及有机酸的加标回收率在91.6%～100.0%之间,乙二醇含水料直接测定无机阴离子的加标回收率在91.8%～104.8%之间.     

离子色谱法测定酒中叠氮根离子

建立了一种测定酒中叠氮化物的离子色谱方法(IC)。样品经稀释、过滤后,依次过OnGuard RP柱和OnGuard Na柱以除去疏水性物质和重金属离子的干扰。以KOH梯度淋洗,淋洗液流速为1.0 mL/min,采用DionexIonPacAS18色谱柱分离,IonPac TAC-UPL1预浓缩富集进样,最后用DS6电导检测器检测,外标法定量。N3-的线性范围为0.005~0.5μg/mL,线性相关系数为0.9998,加标回收率为88%~106%,检出限为0.002μg/mL(以信噪比S/N=3计),相对标准偏差为0.1%~0.6%。     

离子色谱法测定威力酸中的有机酸

采用离子排斥分离,电导检测模式,对威力酸中的4种有机酸成份进行分离测定。将威力酸样品通过萃取、洗涤、过滤之后进样,可以测定其柠檬酸、乳酸、苹果酸、富马酸4种有机酸,在一定的色谱条件下,4种阴离子都具有很好的线性和较低的检出限。威力酸中的柠檬酸,乳酸,苹果酸,富马酸的检出限分别是0.10、0.14、0.30和0.12μg/L,线性相关系数r2在0.9997~0.9999范围内,样品中待测离子峰面积的RSD在4.3%以下(n=10),回收率在94%~105%之间。采用抑制电导的离子色谱法是分析威力酸中的有机酸成份的高效与准确的方法。     

离子色谱法检验尸体心血中草甘膦

建立了离子色谱检测人血中草甘膦的方法。血液样品使用乙腈沉淀蛋白质,离心后取上清液过Dionex OnGuard II RP 柱和Dionex OnGuard IIAg柱后,经IonPac AS-19阴离子色谱柱(25 mm×4 mm)分离,用KOH淋洗液自动发生器(EG)进行梯度淋洗,抑制器采用外加水模式,电导检测器检测。结果表明,草甘膦在10～100 mg/L范围内线性关系良好(相关系数r2=0.9999)。以信噪比(S/N)为3确定方法检出限为0.12 mg/L,以S/N=10确定方法定量限为0.39 mg/L;方法回收率为95.2%～109.1%,相对标准偏差(n=5)为1.2%～3.7%,检测实发案件中死者心血中草甘膦质量浓度为508 mg/L。该方法操作简便,结果准确,适用于血中草甘膦的定量检测,能快速为案件的侦破提供可靠的线索和依据,可满足公安工作的需要。     

Determination of glyphosate by ion chromatography

An ion chromatography system for the determination of glyphosate was described. Ion chromatograph was carried out by suppressed conductivity detection (DX-100). The eluent contained 9 mmol l⁻¹ Na₂CO₃ and 4 mmol l⁻¹ NaOH. The detection limit was 0.042 μg ml⁻¹ (S/N=3). The relative standard deviation was 1.99% and the correlation coefficient of the calibration curve for area was 0.9995. The linear range was 0.042100 μg ml⁻¹. Common inorganic ion and organic acids did not interfere. The recovery was 96.4103.2%. The method was simple, rapid, reliable and inexpensive.     

Determination of levels of adenosine phosphates in blood by ion chromatography

A new method was developed for simultaneous determination of levels of AMP,ADP and ATP in blood by anion-exchange chromatography.The three adenosine phosphates were separated by Dionex IonPac AG18(50 mm×4 mm) guard column and IonPac AS 18(250 mm×4 mm) analytical column using a gradient method and detected with a suppressed conductivity detector. The detection limits(S/N=3) of AMP,ADP and ATP were 38,47,108 ng/L,respectively.The relative standard deviations of retention time,peak area and peak height were all less than 1.87%and a good linear relationship was obtained.This method was applied to analyze human blood samples.     

离子色谱法检测盐酸头孢吡肟中的N-甲基吡咯烷

建立了一种盐酸头孢吡肟中的N-甲基吡咯烷的离子色谱分析方法.采用阳离子交换柱IonPac CS12A作分析柱,甲烷磺酸-乙腈为淋洗液,外加水电抑制模式,电导检测,在10 min内即可完成分析.线性良好(r2=0.9985),样品的RSD在5%以下(n=6),回收率在89.5%～108.4%之间.方法可在盐酸头孢吡肟产品的检验中发挥作用.     

离子色谱法检测幼兔尿样中的乳果糖与甘露醇

测定尿液中乳果糖(L)、甘露醇(M)的含量以及乳果糖/甘露醇排除率(L/M)可以检测肠道通透性,评估肠粘膜屏障功能。采用离子色谱法检测幼兔尿样中的乳果糖和甘露醇,并运用MATLAB软件对数据进行微分处理计算,得出样本中乳果糖和甘露醇的含量以及乳果糖/甘露醇排除率(L/M)。     

离子色谱法检测酸性镀铜液中的微量氯离子

采用Na2CO3-NaHCO3为淋洗液和抑制电导检测,对酸性镀铜液中的微量氯离子进行检测。采用AgNO3作为沉淀剂使Cl-分离富集,再用Na2S2O3溶液溶解沉淀后进行检测,可以很好地消除酸性电镀液中高浓度SO4^2-的干扰。该方法线性良好,Cl^-的检出限为0.01μg/mL,回收率在98.6%-101.7%之间,由于该方法能够很好地消除大量SO4^2-的干扰,在电镀铜工业中对酸性镀铜液中氯离子的监控可发挥作用。     

Determination of anions in lithium-ion batteries electrolyte by ion chromatography

A sensitive and accurate method based on ion chromatography was established for determination of five lithium salts in lithium-ion batteries electrolytes. Chromatographic analyses were carried out on an anion exchange column at flow rate of 1 m L/min. Under the optimal conditions, five target anions(BF_4~-,PF_6~-, TFSI~-, BOB~-and FSI~-) exhibited satisfactory linearity with a correlation coefficient of 0.9996. The relative standard derivations of the target anions were less than less than 0.94%(n = 7). The limits of detections were in the range of 0.068–0.29 mg/L with average spiked recoveries ranging from 96.8% to 105.1%.     

离子对分离和抑制电导检测法测定四乙基铵和四丁基铵根离子

建立了季铵盐的离子色谱分析方法.采用Dionex DX-500 型离子色谱仪,C18柱,电导检测器,以30%乙腈和10 mmol/L甲烷磺酸混合溶液为流动相,流量为1.00 mL/min.四乙基溴化铵和四丁基溴化铵的质量浓度和峰面积的相关系数分别为0.9996和0.9994;线性范围分别为10～80 mg/L和20～120 mg/L;检出限分别为0.28和0.76 mg/L;RSD分别为1.3%、 2.5%.该方法可用于分析水溶液中季铵盐的含量.     

离子色谱法测定塑胶场地中甲苯二异氰酸酯

研究了离子色谱-紫外检测法测定塑胶场地样品中的甲苯二异氰酸酯,先将甲苯二异氰酸酯(TDI)水解成甲苯二胺,用CS12A作分离柱,6%CH3CN 20 mmol/L Na2SO4 18 mmoL/L H2SO4的混合液作淋洗液,紫外波长设置为212nm。测定了样品中的TDI,该方法与直流安培检测相比基线更平直,有更好的线性及相对标准偏差,方法的相关系数为0.9994,检出限为8.0μg/L,回收率为110%。     

N-arylation of azaheterocycles with aryl and heteroaryl halides catalyzed by iminodiacetic acid resin-chelated copper complex

<正>Iminodiacetic acid resin-chelated copper(Ⅱ) complex is effective in cross-coupling reactions between azaheterocycles and aryl or heteroaryl halides,providing N-arylated products in good to excellent yields.The copper catalyst is air stable and can be readily recovered and reused with minimal loss of activity for three runs.