Densitometric Determination of Hecogenin from Agave americana Leaf Using HPTLC

We report a simple TLC densitometric method for the quantification of hecogenin from the leaves of Agave americana using HPTLC. The method was validated for precision, repeatability and accuracy. The method was found to be precise with RSD of 0.78 (intraday) and 0.82 (interday) for different concentrations of hecogenin. Instrumental precision was 0.42 (% RSD) for hecogenin. The content of hecogenin in different samples was estimated by the proposed method and was found to be in the range of 0.05−0.14% w/w in the samples analysed. Accuracy of the method was checked by conducting recovery study at three different levels for hecogenin and the average percentage recovery was 98.98%, 101.92% and 103.33%, respectively. The TLC densitometric method developed for the quantification of hecogenin was found to be simple, precise, specific, sensitive, accurate and can be used in routine quality control. Revised: 7 and 25 April 2006     

Identification of chlorinated sulfur compounds in pulp mill effluents by GC-MS and GC-AED

Summary Three chlorinated dimethyl sulfones and five chlorinated thiophenes have been identified in the alkaline extraction liquor from a bleach plant by gas chromatography with atomic emission detection (GC-AED) and with mass spectrometry (GC-MS). The information on elemental content obtained by GC-AED enabled a rapid screening of the sulfur compounds and provided important structural information complementary to the mass spectral data. Quantitation was accomplished by GC-AED based on universal calibration.     

Electroanalytical and chromatographic determination of pentachlorophenol and related molecules in a contaminated soil: a real case example

Electroanalytical and chromatographic methodologies have been applied for the determination of pentachlorophenol (PCP) and some of its derivatives in real soil samples contaminated by industrial discharge. The analytes were extracted with hexane from soil samples collected at different points of the site and mixed to produce a representative sample. Square wave voltammetry (SWV) experiments were carried out on either a boron-doped diamond (BDD) electrode or a gold ultramicroelectrode (Au-UME) in an analyte composed by the Britton-Robinson (B-R) buffer at pH 5.5 with the direct addition of proper amounts of the extract. The voltammetric responses revealed an irreversible anodic peak at approximately 0.80 V vs. Ag/AgCl with a peak current showing a linear dependence on PCP concentration. This linear relationship yielded a detection limit (DL) of 2×10⁻⁸ mol l⁻¹ (or 5.5 μg l⁻¹) for the BDD electrode and 6.9×10⁻⁸ mol l⁻¹ (18.4 μg l⁻¹) for the Au-UME, while the independently measured HPLC detection limit was 1.1×10⁻⁸ mol l⁻¹ (3.0 μg l⁻¹). The application of electroanalytical and chromatographic methodologies in the analysis of soil extracts revealed, besides the PCP responses, signals for some related molecules such as o-tetrachlorobenzoquinone (o-chloranil), hexachlorobenzene and tetrachlorophenol. Recovering experiments for PCP showed a concentration of 27.5 mg kg⁻¹ for the electroanalytical determinations and 26.8 mg kg⁻¹ for the HPLC analysis, values exceedingly high if considering that the maximum residue limit established for natural waters by the Brazilian Environmental Agency is 10 μg l⁻¹.     

顶空气相色谱法测定延生护宝液中甲醇残留量

本文用顶空气相色谱法，以ＧＤＸ－１０１为固定相，测定了延生护宝液中甲醇残留量，方法的回收率在８５．９％－１０１．６％之间，变异系数０．３％，最小检出量１．０ｍｇ／Ｌ。     

Simultaneous separation and identification of hashish constituents by coupled liquid chromatography-mass spectrometry (HPLC-MS)

Summary This paper reports the use of liquid chromatography for the separation and determination of the major cannabinoids extracted from hashish samples. The direct coupling to the mass spectrometer enables the selective identification both of neutral and acidic cannabinoids. The developed method does not require any preliminary derivatization and should, therefore, be of interest in forensic analysis for simple and unequivocal determination of hashish constituents.Part of this work was presented at the 2nd Italian-Spanish Joint Meeting of Medicinal Chemistry, 30 August–3 September 1995, Ferrara, Italy.     

舒兰褐煤树脂组分中某些分离物的化学研究

我国褐煤资源丰富 ,分布于云南、吉林、黑龙江、山东和内蒙古等地。褐煤除作燃料和腐植肥料外 ,还应用于轻化工和机械工业 ,如从褐煤制取褐煤蜡。褐煤蜡中含有较多的树脂物质 ,影响了褐煤蜡的质量 ,因此通常褐煤蜡树脂作为废弃物脱除 ,以提高褐煤蜡的质量。褐煤蜡的化学组成为纯蜡和树脂 ,前者为高碳脂肪酸和脂肪醇的酯类、游离脂肪酸和脂肪醇 ,以及烃类物等 ;后者则以萜类为主 ,并含有甾醇、羟基酸和烃化合物[1～ 5] 。 1982年唐运千等采用红外光谱和氢核磁共振谱检定 ,褐煤树脂中含有 β 谷甾醇 ;柱层析和薄层层析检出雌二醇和雌酚酮[2 ] …     

用铜（Ⅱ）—L—精氨酸配体交换薄层色谱拆分氨基酸对映体

报道了一种新的配体交换薄层色谱拆分氨基酸对映体的方法。以醋酸铜－Ｌ－精氨酸的络合物为配体交换剂，用浸渍的方法吸附在硅胶薄层板上，制成配体交换薄层，用ＰＲＩＳＭＡ优化法选择出展开剂的最佳组成为：甲醇／乙腈／四氢呋喃／水＝８０：８．２：５．８：６，在此色谱条件下，十对氨基酸对映体得到良好的分离，Ｄ－和Ｌ－氨基酸的相对比移值在１．０９－２．４０之间。文中对配体交换薄层的制备方法，样品的分子结构及色谱行为