气相毛细管色谱法测定油酸

用甲醇－硫酸将油酸衍生为脂肪酸甲酯，用自制、耐高温气相毛细管柱分离测定，建立了快速分离测定油酸的方法。方法准确可靠、分析速度快。

GC-MS Analysis of Essential Oil Constituents from Rhizome and Root of Notopterygium forbesii

Aim To analyse the chemical constituents of the essential oil extracted from the rhizome and root of Notopterygium forbesii Boiss. and provide scientific basis for quality control. Methods The total essential oil was extracted by water-steam distillation and separated by capillary gas chromatography (GC). The components were determined by normalization method, and identified by GC-MS. Results GC-MS exhibited 217 peaks and 100 compounds were identified, accounting for 78.3% of the total essential oil. Conclu...

GC-MS Analysis of Essential Oil Constituents from Buds of Tussilago farfara L.

Aim To analyse the constituents of the essential oils extracted from the buds of Tussilago farfara L. in the GAP Bases of Traditional Chinese Medical Materials and provide scientific basis for quality control. Methods The essential oils were extracted by water-steam distillation and separated by GC capillary column chromatography. The components were quantitatively determined by normalization, and identified by GC-MS. Results GC-MS exhibited 259 peaks and 65 compounds were identified, accounting for 84.62% of the total essential oil. Conclusion In the total essential oil contained in the buds of Tussilago farfara L., copaene （2.36%）, （ ＋ ） -Epi-bicyclosesquiphellandrene （ 3.91% ）, γ- elemene （2.18%）, fl-bisabolene （ 13.93% ）, spathulenol （ 3.44% ） as the sesquiterpenes and its derivatives, and 1-undecene （4.83%）, （ E）-cycloundecene （8.49%）, bicycle [ 10. 1.0] tridec-l-ene （ 1. 45% ）, 1-tridecene （3.44%）, （Z）-7,11-dimethyl-3-methylene-1,6,10-dodecatriene （2.66%）, 1- pentadecene （4.57%）, [ 1R-（ 1R^＊, 4Z, 9S^＊ ） ]-4,11,11-trimethyl-8-methylene-bicyclo [ 7.2.0] undec-4-ene （ 1.03% ）, 6,6-dimethyl-2-methylene-7-（ 3-oxobutylidene ）-oxepan-3-ylmethyl acetic acid ester （2.02%）, 1, E-11, Z-13-heptadecatriene （ 3.72% ）, （ Z, Z, Z） -9,12,15-octadecatrien-l-ol （ 1.85% ）, 3,7,11-trimethyl-dodeca-2,4,6,10-tetraenal （ 1.31% ）, n-hexadecanoic acid （ 3.12% ） , （Z, Z） -9,12-octadecadienoic acid （2.26%）, （ Z, Z, Z） -9,12,15-octadecatrienoic acid methyl ester （ 1.12% ） , heneicosane （ 1.82% ）, and pentacosane （ 1.03% ） are the main components.

GC-MS Analysis of Essential Oil Constituents from Rhizome and Root of Notopterygium incisum

Aim To analyse the chemical constituents of the essential oil extracted from the rhizome and root of Notopterygium incisum Ting ex H.T. Chang, providing scientific basis for quality control. Methods The total essential oil was extracted by water-steam distillation and separated by capillary gas chromatography （GC）. The components were determined by normalization method, and identified by GC-MS. Results GC-MS exhibited 242 peaks and 83 compounds were identified, accounting for 75.77% of the total essential oil. Conclusion In the total essential oil of the rhizome and root of N. incisum, monoterpenes and sesquiterpenes accounted for 13.63% and 67.93%, respectively, in which （ 1S）-β-pinene （ 1.67% ）, 3-carene （ 1.05% ）, limonene （ 1.22% ）, and 1S-endo-bornyl acetate （ 1.68% ） as the monoterpenes and its derivatives, and （ ＋ ） -β-elemene （6.78%）, sativene （1.54%）, α-caryophyllene （2.64%）, germacrene D （1.67%）, eudesma-4 （ 14 ）, ll-diene （2.36%）, α-selinene （2.42%）, δ-cadinene （ 1.55% ）, 3,7,11-trimethyl-2,6,10-dodecatrien-1-ol （1.03%）, （ ＋ ）-elemol （5.18%）, （-）-spathulenol （1.40%）, guaiol （3.81%）, dehydroxy-isocalamendiol （ 1.06% ）, γ-eudesmol （ 1.05% ）, α-eudesmol （7.97%）, bulnesol （3.09%）, and carotol （2. 30% ） as the sesquiterpenes and its derivatives were main components. In addition, isopropyl transcinnamate was the maximum compound （ 11.3% ） of the total essential oil.

Determination of Dichlofluanid Residue in Soybean by Capillary Collumns Gas Chromatography

A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with N-hexane,and then they were cleanup with column that filled with florisil,subsequently separated by Capillary Column Gas Chromatography,and the electron capture detector （ECD） was used for detection.The detection limit of this method was 0.005 mg/kg （S/N=3）,and this method was rapid,sensitive and accurate,and was applied in the determination of dichlofluanid residue in soybean.

Separation Properties of a New Polysiloxane-Anchored β-Cyclodextrin Derivative as Gas Chromatography Stationary Phase

A new capillary gas chromatography stationary phase, monokis (2,6 di O benzyl 3 O propyl (3’)) hexakis(2,6 di O benzyl 3 O methyl) β CD bonded polysiloxane, was synthesized. It exhibited separation abilities to disubstituted benzene isomers and some chiral solutes. It was also found that the polarity of CD derivatives can be lowered both by chemically bonding it to polysiloxane and by diluting it in polysiloxane. The separation abilities of the polysiloxane anchored CDs (SP CD) are higher than that of the unbonded CDs (S CD) and the diluted S CD at lower column temperature. Hydrosilylation reaction is one of the best methods to lower the operating temperature of CDs.

Application of Multicapillary Column to High Speed GC Separation of Industrial Chemicals

Two multicapillary coluumns(SE 30 and Carbowax 20M)were used for high speed GC separation of positional isomers of industrial chemicals The performances of the two multicapillary columns were also evaluated,such as the effects of carrier velocity,column temperature and sample capacity Two typical explosive isomers(DNT and TNT)were well separated on SE 30 multicapillary column,while some important chemicals(e g xylenes,xylenols)were separated on Carbowax 20M multicapillary column at high speed The multimulticapillary column shows the feature of fast analysis,relatively lower column temperature and larger sample capacity

Enantioselective Determination of R-(-)-and S-(+)-Mexiletine in Microsomal Incubates by Capillary gas Chromatography

A method for the assay of R ( ) and S (+) mexiletine in rat liver microsomal incubates was developed. The method involved extraction of mexiletine from the microsomal incubates, and formation of mexiletine diastereomeric derivatives with a chiral reagent S ( ) N trifluoroacetyl prolyl chloride. Separation and quantitation of the diastereomeric mexiletine derivatives were carried out by a capillary gas chromatographic system with flame ionization detection. The assay was linear from 5 to 500 μg/ml for each enantiomer. The average recoveries of analytical method were 93 31±5 59% and 93 10±5 11% for R ( ) and S (+) mexiletine, respectively. The limits of detection and quantitation for the method were 1 0 μg/ml and 5 0 μg/ml for the R ( ) and S (+) mexiletine isomers, respectively. The reproducibility in the assay was better than 16.5% (RSD). The method has been applied to the metabolism study of R ( ) and S (+) mexiletine in rat liver microsomal incubates.

Cross-Linked Crown Ether-SE-54 as Stationary Phase for Open-Tubular Column Gas Chromatography

The cross-linking of crown ether-SE-54 in fused-silica capillary columns were initiated by dicumyl peroxide(DCUP),azo-bis-isobutyronitrile (AIBN)and ozone(O_3).Parameters of evaluation such as polarity,selectivity, phase transition temperature and thermal stability were studied and compared with those of poly(crown ether)stationary phase.

Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco

Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described.The determination was carried out by capillary gas chromatography(GC) with electron capture detection(ECD) and confirmed by GC-MS.The mean recoveries and relative standard deviation(RSD) were 93.2%～112.9% and 3.5%～6.7%,respectively at levels ranging from 0.01 to 0.1 mg/kg.The limit of determination was 0.001 mg/kg.Tobacco samples in routine check were successfully analyzed using the proposed method.

Identification of Blood Serum Lipid Compositions Isolated from Diabetic PatientsmType II Treated with Polyherbs by Capillary Gas.Chromatography

This study included treatment of diabetic patients--type II with a polyherbs containing Nigella sativa, Trigonell foenum-graceum, Cyperus rotundus, Teucrium polium divided into two groups, first group was taken herbs with chemical treatment （drugs） and the other group which used herbs only. These groups were compared with healthy persons as a control group. Separation of the lipid component containing in the serum of two groups under study for diabetes mellitus patient--type lI before and after treatment with polyherbs by patients were performed. The separation of the components of different kinds of lipid parts like cholesterol ester （CE）, triglyceride and phospholipids, in the blood using thin layer chromatography （TLC） and capillary gas chromatography （CGC）. The results of this study for ester cholesterol part of serum patients show that there was a significant increase in the percentage of saturated fatty acid （SFA） and monounsaturated fatty acid （MUFA） before the treatment of the two groups compared to the control group and a significant decrease was observed in the percentage of these fatty acid after the treatment by polyherbal mixture than the percentage before treatment. Also, the results for the same part of ester cholesterol serum were showed a significant decrease in percentage of polyunsaturated fatty acid （PUFA） in the two groups of diabetes mellitus patients in comparison with the control group and there were a significant increase observed in PUFA percentage after the treatment. For triglyceride part in serum lipid, the results of this study were shown that there was a significant increase in percentage of SFA and PUFA before treatment in comparison with control group and after treatment for three months of the two groups of patients, shows a significant decrease in SFA but an increase in the percentage of PUFA was observed than that observed before treatment, also, there was a significant decrease in MUFA before treatment comparison with control group, while there was a significant increase which was observed after treatment in a percentage for the two groups of triglyceride part in serum lipid. The results indicated that there was a significant decrease in percentage of SFA before and after also in MUFA after the treatment in both groups compared with control and a significantly increase in PUFA percentage was also shown for phospholipids part in the serum.