HPLC/MS测定蒲公英颗粒中绿原酸、咖啡酸和阿魏酸的含量

建立了同时测定蒲公英颗粒中绿原酸、咖啡酸和阿魏酸3种酚酸物质含量的HPLC-MS方法.样品用含5%甲酸的甲醇溶液超声提取后,在Zorbax Eclipse XDB-C18(2.1mm×150mm,5μm)色谱柱上,以含0.2%甲酸的水(A)-乙腈(B)体系为流动相,进行梯度洗脱,线性梯度洗脱程序为:Omin,5%B;1.5min,10%B;10min,40%B;流速:0.25mL/min;在ESI正离子模式下,采用选择性离子监测方法进行检测.结果显示,绿原酸、咖啡酸和阿魏酸的线性范围分别为0.050～20.0、0.030～20.0和0.100～20.0μg/mL,检出限分别为0.010、0.006和0.020μg/mL.平均加标回收率为96.4%～101.6%,相对标准偏差为1.7%～3.3%.样品在10 h内测定基本不变,可用于蒲公英颗粒的质量控制.     

高效液相色谱法同时测定忍冬中7种成分

建立了在不同时间段内转换使用不同波长同时测定忍冬花和叶中7种化学成分(绿原酸、咖啡酸、芦丁、木犀草苷、异绿原酸A、异绿原酸B、异绿原酸C)的高效液相色谱分析方法,同时应用该方法分析了忍冬花、忍冬老叶和新叶中成分含量的差异。色谱柱为Agilent Eclipse Plus C18(250 mm×4.6 mm, 5 μm);流动相为0.3%甲酸水溶液(A)和乙腈(B),梯度洗脱,流速1 mL/min;采用VWD紫外检测器转换波长(330 nm、350 nm)检测。应用所建立的方法测定忍冬新叶中绿原酸、木犀草苷含量分别为2.572%、1.498‰,均比药典中规定的含量高,有必要进一步的研究和开发利用。该方法准确、简便、灵敏度高,适用于忍冬中7种化学成分含量的同时测定和忍冬的质量控制及综合评价。     

高效液相色谱-电喷雾离子阱质谱联用法测定金银花中绿原酸和咖啡酸

建立了高效液相色谱-电喷雾离子阱质谱法(HPLC-ESI-ITMSn)同时测定了金银花中绿原酸和咖啡酸活性成分的分析方法。样品用体积分数80%乙醇回流提取,用Zorbax Eclipse XDB-C18柱分离,以体积分数0.5%甲酸的乙腈-甲酸水溶液为梯度流动相,以保留时间和质荷比对分离出的组分予以定性确证,用峰面积进行定量。绿原酸和咖啡酸的线性范围均为10.0~1000.0μg/L,检出限(以信噪比为3计)均为2.0μg/L。样品的加标平均回收率为92.7%~98.7%,相对标准偏差为1.4%~2.7%。该方法适用于其它复杂体系中绿原酸和咖啡酸的分析。     

枸杞润肤霜中两种酚酸类成分的高效液相色谱检测及质谱确证

建立了自制枸杞润肤霜中绿原酸和咖啡酸的高效液相色谱分析及液相色谱-串联质谱确证方法。枸杞润肤霜样品经甲醇超声提取,提取液离心处理后,取上清液经微孔滤膜过滤后测定。采用Aglient HC-C18色谱柱(250×4.6mm,5μm)分离,以甲醇-0.5%乙酸水溶液(27∶73,V/V)为流动相,等度洗脱,流速1.0mL/min,检测波长327nm。绿原酸、咖啡酸分别在3.3~250μg/mL、3~225μg/mL间线性关系良好(r=0.9993);平均加标回收率分别为98.28%、99.26%,相对标准偏差(RSD)均为1.93%。自制枸杞润肤霜中绿原酸、咖啡酸含量分别为0.0398 mg/g、0.0323mg/g。该方法快速、准确,适用于同时测定枸杞润肤霜中绿原酸、咖啡酸的含量。     

高效液相色谱-二极管阵列检测-电化学检测联用技术同时测定三精双黄连口服液中的4种化合物

建立了应用高效液相色谱-二极管阵列检测-电化学检测(HPLC-DAD-ECD)联用技术同时测定三精双黄连口服液中的绿原酸、咖啡酸、黄芩甙和木樨草素的方法。以Zorbax SB-C18柱(150 mm×4.6 mm i.d., 5.0 μm)为色谱柱,柱温为30 ℃，流动相为(A)甲醇和(B)甲醇-水-冰醋酸(体积比为50∶50∶1),其梯度洗脱程序为2%A3 min3%A12 min25%A5 min80%A。流速为0.8 mL/min。二极管阵列检测波长为275 nm。电化学单安培检测器的工作电压为0.7 V。在上述条件下实现了绿原酸、咖啡酸、黄芩甙和木樨草素的分离检测。上述4种化合物的回收率为96.6%～99.6%,相对标准偏差(RSD)为2.5%～4.1%,检测限依次为1,0.2,9和7 mg/L。该方法简便、快速,重现性和准确度较好,可作为测定双黄连口服液中绿原酸、咖啡酸、黄芩甙和木樨草素的有效方法。     

高效液相色谱-串联质谱法分离鉴定绿原酸及其相关杂质

建立了高效液相色谱-串联质谱法（HPLC-MS/MS)分离和鉴定绿原酸及其相关杂质的方法。采用C18色谱柱(5 μm,4.6 mm×150 mm),乙腈-水（含0.1%甲酸）(体积比为8∶92)为流动相,经HPLC-MS/MS和HPLC-二极管阵列检测器在线检测,对工业绿原酸中的奎尼酸、咖啡酸、绿原酸同分异构体等8个相关杂质的结构进行了鉴定。     

高效液相色谱法同时测定苹果汁中6种酚类物质

建立了同时测定苹果汁中儿茶素、绿原酸、咖啡酸、表儿茶素、香豆酸和阿魏酸6种酚类物质的反相高效液相色谱方法,并对酚类物质的稳定性进行了探讨。选用Eclipse XDB-C18色谱柱(150 mm×4.6 mmi.d,5μm),以甲醇-1%乙酸水溶液作为流动相进行梯度洗脱。柱温30℃,流速1.0 mL/min,在280 nm波长下进行检测。本方法样品处理简单,具有良好的重现性和线性,相关性系数均达到0.9999,儿茶素、绿原酸、咖啡酸、表儿茶素和香豆酸和阿魏酸的回收率分别为102%~103%、94.3%~101%、102%~104%、98.4%~101%、96.2%~99.8%和102%~104%;检出限分别为20、30、10、20、7和15μg/L(S/N=3)。     

反相高效液相色谱法快速测定大麦籽粒中13种酚酸类化合物

建立了快速测定大麦籽粒中13种酚酸类化合物(没食子酸、原儿茶酸、绿原酸、对羟基苯甲酸、咖啡酸、香草酸、丁香酸、间羟基苯甲酸、对香豆酸、阿魏酸、藜芦酸、邻香豆酸和水杨酸)的反相高效液相色谱方法.采用SUPELCOAscentis(@) C18色谱柱(150 mm×4.6 mm,5μm)分离,流动相为甲醇-0.1％甲酸水溶...     

高效液相色谱法同时检测黄酒中的5-羟甲基糠醛和9种多酚

建立了黄酒中5-羟甲基糠醛和9种多酚(儿茶素、表儿茶素、绿原酸、芦丁、咖啡酸、原儿茶酸、丁香酸、阿魏酸、p-香豆酸)的高效液相色谱检测方法。采用Diamonsil C18柱(150mm×4.6mm,5μm)分离,柱温为42℃,检测波长为280nm,流动相为乙腈和3%乙酸水溶液,梯度洗脱,20min内10种物质得到了较好的分离。各化合物回归方程的相关系数r为0.9911～0.9995,检出限为0.2～0.5mg/L;相对标准偏差RSD≤2.4%;10种组分的平均回收率为89.4%～98.3%;能够满足定量分析要求。实验结果表明,本方法适用于不同种类和年份黄酒中5-羟甲基糠醛和9种多酚的检测。     

高效液相梯度洗脱法测定杏香兔耳风中绿原酸和芦丁

建立了反相高效液相色谱法同时测定不同来源的杏香兔耳风中的绿原酸和芦丁。采用Kromasil C18柱(4.6 mm i.d.×250 mm,5μm),以甲醇-0.5%H3PO4的水溶液为流动相,梯度洗脱程序为0 min(30∶70)-15 min(30∶70)-20min(50∶50)-40 min(50∶50);流速0.8 mL/min;检测波长350 nm;柱温25℃;光电二极管阵列检测器(PAD)。绿原酸线性范围为0.654~5.886μg,r=0.9997,样品的平均加标回收率为98.6%,RSD 1.7%;芦丁线性范围为0.218~1.962μg,r=0.9993,样品的平均加标回收率为97.1%,RSD 2.3%。本法可作为杏香兔耳风中绿原酸和芦丁的定量分析方法。     

电堆集富集非水毛细管电泳同时测定水杨酸、肉桂酸、阿魏酸和香草酸

建立了同时分离测定水杨酸、肉桂酸、阿魏酸和香草酸的电堆集富集-非水毛细管电泳(NACE)的新方法。运行缓冲溶液为40mmol/L乙酸钠-2.5mmol/L氢氧化钠甲醇溶液,电压-25kV,在225nm波长下紫外检测。对电压、乙酸钠浓度、氢氧化钠浓度、进样时间、样品溶液等因素对电堆集及分离的影响做了系统的研究。水杨酸、肉桂酸、阿魏酸和香草酸分别在1.4~28mg/L、0.40~8.0mg/L、0.7~18mg/L和0.7~30mg/L范围内线性关系良好(r=0.9999、r=0.9997、r=0.9994、r=0.9997);回收率分别为95.8~99.6%、96.2~98·2%、95.7~105%和98.9~103%,基于3倍信噪比(S/N=3),4种有机酸的检出限分别为0.069、0.051、0.107和0.089mg/L。     

离子色谱法测定乙醛酸中的顺丁烯二酸和乙二酸

采用抑制电导离子色谱法测定高浓度乙醛酸基体中痕量的顺丁烯二酸和乙二酸。将乙醛酸样品稀释至1 000倍体积后,采用高浓度的淋洗液,以高容量色谱柱对样品进行分析。实验结果表明,顺丁烯二酸和乙二酸最低检出限分别为12.7,19.6μg/L,重现性(n=5)分别为1.13%,1.11%,回收率分别为97.9%,94.7%。该方法具有较高的灵敏度,适用于乙醛酸的例行检测。     

Determination of Cyanuric Acid or Trichloroisocyanuric Acid in Air

Abstract

An analytical procedure for measurement of cyanuric acid or trichlor oisocyanuric acid in air has been developed. The procedure involves air sampling with a 37-mm PVC membrane filter, recovery with a phosphate buffer, and analysis by high performance liquid chromatography with a UV detector at 225 nm. The interior surface of the front piece of the cassette filter holder also is analyzed. Average recoveries were 0.98 to 1.00 after fortification of PVC filters with 12- to 412-μg quantities of cyanuric acid. Average recoveries of trichloroisocyanuric acid were 0.83 to 0.98 after fortification of glass surfaces with 12- to 424-μg quantities (these are reasonable approximations for recoveries of trichloroisocyanuric acid from PVC filters). The analyst should ascertain which analyte is present at the sampling site because trichloroisocyanuric acid reacts with water in the phosphate buffer to form cyanuric acid in high yield.     

对氨基苯甲酸的合成研究进展

综述了以对硝基苯甲酸为原料合成对氨基苯甲酸的近期研究进展。并从技术和经济角度讨论了各种合成方法的优点与不足。     

以对甲基苯磺酸作为淋洗液用离子色谱法测定酸雨中的有机酸

本文研究了用对甲基苯磺酸作为淋洗液测定液相中HCOO~-和CH_3COO~-的离子色谱条件,该方法对HCOO~-和CH_3COO~-的最低检出限分别为48ppb和93ppb。该方法与用进口的辛磺酸作为淋洗液的方法进行了对比实验,并用于两广实际酸雨样品中甲酸和乙酸的测量。     

Surface Functionalization of Magnetite Nanoparticles with Sulfonic Acid and Heteropoly Acid: Efficient Magnetically Recoverable Solid Acid Catalysts

New magnetically recoverable solid acid catalysts for acid‐catalyzed reactions were designed via the surface chemical functionalization of silica‐coated magnetite nanoparticles (SCMNPs) with sulfonic acid groups. First, the SCMNPs were covalently functionalized with 3‐aminopropyl groups to achieve Amp‐SCMNPs. Then, reaction of the Amp‐SCMNPs with 1,4‐butane sultone followed by acidification with phosphotungstic acid (HPW) or diluted sulfuric acid produced magnetically recoverable solid acid catalysts, HPW‐ampsul‐SCMNPs and H‐ampsul‐SCMNPs, respectively. Both catalysts were characterized by various physicochemical analyses such as Fourier transform infrared (FT‐IR) and inductively coupled plasma‐optical emission (ICP‐OES) spectroscopies, vibrating sample magnetometry (VSM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), and energy‐dispersive X‐ray (EDX) analyses. Finally, the catalytic activities of the prepared catalysts were examined in the esterification of acetic acid with butanol and acetalization of benzaldehyde with ethylene glycol. Excellent catalytic efficiencies were obtained in both cases. The catalysts were consecutively recovered and reused five times without significant loss of their activities.     

Mechanochemical Complexation between Deoxycholic Acid and Salicylic Acid

A complex between deoxycholic acid (DCA) and salicylic acid (SA) was prepared by grinding and coprecipitation methods. The resultant complex was characterized by means of powder X-ray diffractometry, IR spectroscopy and thermal analysis. The stoichiometry (DCA : SA 1 : 1) of the complex obtained by grinding was identical to that obtained by coprecipitation. The powder X-ray diffraction pattern of the DCA–SA complex differed from the typical pattern of DCA–guest complexes such as DCA–camphor and DCA–phenanthrene complexes. IR spectra suggested that a different kind of hydrogen bonding was formed in the crystal of the DCA–SA complex, compared with the other DCA–guest complexes. This was in good agreement with data from the crystal structure.     

硝酸氧解法提高泥炭中黄腐酸的产率

硝酸氧解法提高泥炭中黄腐酸的产率;腐植酸;硝酸氧化降解     

Determination of Monochloroacetic Acid and Dichloroacetic Acid for Quality Control of Acetic Acid Chlorination Industry by Ion Chromatography

An ion chromatographic method is described for the purpose of quality control in the process of monochloroacetic acid production. Using 2.5 mM NaOH–10% methanol as eluent, the simultaneous determination of acetic acid, monochloroacetic acid, dichloroacetic acid, and Cl⁻ was obtained in a single run. Monochloroacetic acid and dichloroacetic acid showed good linearity in the range 0.1–20 and 0.15–20 μg/ml and correlation coefficients were 0.9999 and 0.9998, respectively. The detection limits (signal-to-noise ratio 3:1) of monochloroacetic acid and dichloroacetic acid were 17 and 25 ng/ml. This simple, sensitive, and time-saving method can be applied for composition analysis in acetic acid chlorination production.