薄层层析-高效液相色谱法测定食品中苏丹红

建立了薄层层析-高效液相色谱联合技术测定食品中违禁添加物苏丹红Ⅰ、Ⅱ的新方法。采用硅胶板将苏丹红与杂质分离,在设定的色谱条件下测得浓度在0.1～20.0μg/mL范围内,峰面积（Y）与浓度（X）呈良好线性关系,苏丹红Ⅰ、的回归方程为Y1=-18785＋138962X,Y2=-2623＋131432X,相关系数R1=0.9997,R2=0.9998。将该法应用于辣椒粉、辣椒油、番茄酱等中的苏丹红Ⅰ、Ⅱ的检测。其检出限分别为0.024μg/g0、.027μg/g。     

高效液相色谱法同时测定吡虫啉和多效唑

采用高效液相色谱法连续测定吡虫啉和多效唑的含量,该方法中吡虫啉和多效唑标准偏差分别为0.94和0.59,变异系数为0.58%和0.45%,在0 8～15 0mg/L和1 5～25mg/L的范围内与峰高呈良好的线性关系,回收率为99 6%和98 9%,其相关线性系数为0 9995和0 9989,满足在水样、秧苗、稻谷样品中的检测要求,方法简便、快速、准确。     

薄层法制备聚天冬氨酸及其阻垢性能研究

以马来酸酐和碳酸铵为原料,通过薄层聚合制备了聚天冬氨酸,研究了反应物配比、聚合时间及反应温度等因素对聚合物产率、相对分子质量的影响;考察了聚合物用量及相对分子质量对阻垢性能的影响.结果显示:碳酸铵和马来酸酐的化学计量数为1.2∶1、反应温度185℃、反应时间50～60 min时,产率可达88%,产物对硫酸钙和碳酸钙均具有良好的阻垢性能.     

Quantitative Determination of Natural Glycolipids from Oil Seed by Automated High‐Performance Thin‐Layer Chromatography (HPTLC)

The role of glycolipids in vegetable oil refining and production of bio‐based fuels has not been disclosed so far. Such investigations required a reliable and reproducible quantitative determination of these compounds. Fundamental data were therefore established on the quantitative determination of glycolipids in vegetable oil gums by means of high‐performance thin‐layer chromatography (HPTLC). Concentrating on five abundant natural glycolipid classes found in these oils, identification of a suitable separation method for the employed glycolipid mixture and those parameters relevant for successful detection were considered in detail. The special importance of sample volume when employing quantitative HPTLC was discussed. Acetone/chloroform/water 6:3:0.4 (v/v/v) was identified as a convenient mobile phase for the investigated issue. A derivatization reagent comprising methanol, copper(II)sulfate pentahydrate, sulfuric acid 98 %, and phosphoric acid 85 % was identified. Subsequent heating at 135 °C for 10 min finished the derivatization and enabled detection at λ = 370 nm. Calibration curves ranging from 1500 to 31.25 ng/mL, regarding both peak area and peak height, were determined. The good correlation of parameters enabled the application of the method to real oil gum samples from sunflower and soybean oil. This revealed that digalactosyldiglycerides in combination with either sterylglucosides or acylated sterylglucosides represented the major glycolipid classes in these oils.     

高效液相色谱法同时测定红景天中维生素D和E研究

用高效液相色谱法首次测定了红景天中维生素D和E的含量。在NOVA -PakC1 8柱上 ,甲醇作流动相 ,紫外检测。实验回收率大于 92 .5 % ,变异系数小于 2 .0 % ,维生素D和E的检出限分别为 1 .0ng ,7.1ng。特征波长的应用 ,使分析方法更为简便、准确。     

SPE-快速分离柱HPLC法测定枸杞样品中的类胡萝卜素

研究了固相萃取(SPE)富集和预分离,快速分离柱高效液相色谱(HPLC)快速测定枸杞样品中类胡萝卜素的新方法;枸杞样品中的类胡萝卜素用W aters Sep-Pak C18固相萃取小柱预分离,然后以ZORBAX Stab leBound(4.6 mm×50 mm,1.8μm)快速分离柱为固定相,甲醇-四氢呋喃为流动相分离,V(甲醇)∶V(四氢呋喃)=80∶20,用二极管矩阵检测器检测,检测波长为450 nm,枸杞样品中的几种类胡萝卜素在5 m in内可达到基线分离,比常规方法节约时间75%左右。方法标准回收率为95%~103%,RSD为1.9%~2.6%。     

基质固相分散-高效液相色谱法测定烟草中的茄呢醇

研究了用基质固相分散-高效液相色谱法测定烟草中的茄呢醇。将m(烟草样品)/m(硅胶)=1∶4充分研磨后装柱,用环己烷-二氯甲烷洗脱样品中的茄呢醇,然后以ZORBAX Stable Bound(4.6×10 mm,1.8μm)C18快速分离柱为固定相,甲醇-四氢呋喃为流动相分离,蒸发光散射检测器检测;样品中的茄呢醇在0.8min内可达到基线分离。方法标准回收率为97%～102%,RSD为1.6%～2.2%。     

四-(对甲基苯基)-卟啉柱前衍生-固相萃取富集高效液相色谱法测定烟草中痕量汞

研究了用四 (对甲基苯基 ) 卟啉柱前衍生 ,固相萃取富集 ,高效液相色谱测定烟草中痕量汞的方法。烟草样品用微波消化后 ,用四 (对甲基苯基 ) 卟啉 (T4 MPP)柱前衍生 ,用WatersSep Park C1 8固相萃取小柱萃取富集汞的T4 MPP络合物 ,然后用甲醇 (内含 0 .0 1mol/L四氢吡咯 醋酸缓冲盐 )和四氢呋喃 (内含 0 .0 1mol/L四氢吡咯 醋酸缓冲盐 )梯度洗脱 ,WatersXterraTMRP1 8(3 .9× 15 0mm)色谱柱作为固定相分离 ,用二极管矩阵检测器检测 ,汞含量在 1～ 12 0 μg/L范围内与峰面积成线性关系 ,根据信噪比 (S/N =3 ) ,方法检测限为 0 .3 μg/L ,方法相对标准偏差在 1.5 %～ 2 .4%之间 ,标准回收率在 94%～ 10 6%之间 ,该方法用于测定烟草中的汞 ,结果满意。     

高效液相色谱法测定烟草样品中的叶黄素和β-胡萝卜素

研究了用固相萃取和高效液相色谱法测定烟草样品中的叶黄素和β 胡萝卜素;烟草样品中的叶黄素和β 胡萝卜素用90%的丙酮震荡萃取,然后用WatersSep Park C18固相萃取小柱预分离和富集,以WaterNova Pak C18色谱柱为固定相,(1+1)甲醇异丙醇溶液 水梯度洗脱为流动相,二极管矩阵检测器检测测定。该方法标准回收率为96%～104%,RSD%为1.26%～2.43%;用于烟草中叶黄素和β 胡萝卜素的测定,结果满意。     

Preparative Purification of the Major Flavonoid Glabridin from Licorice Roots by Solid Phase Extraction and Preparative High Performance Liquid Chromatography

This study investigated a novel, simple, and economical method for the preparation and purification of glabridin from licorice roots. Glabridin was initially obtained from ethyl acetate extraction of licorice, followed by using solid phase extraction (SPE) and preparative high performance liquid chromatography (HPLC). The content of glabridin increased from 0.23% to 35.2% after SPE, and then a 16 mg product at a high purity of over 95% was obtained from 10 g licorice roots after purification by preparative HPLC. The purity was assessed by analytical HPLC, and the purified compound was characterized by LC-MS/MS and ¹H NMR.     

反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸及其主要杂质的含量

建立了反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸和3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯含量方法.甲醇和20 mmol/L乙酸铵(pH 5.0)为流动相,采用HC-C18色谱柱,在波长240 nm处检测.该方法在12.387～1238.7 mg/L 3-二氟甲基-1-甲基-1H...