Novel guanidinium-based ionic liquids as stationary phases for capillary gas chromatography

The present study describes guanidinium-based ionic liquids（GBILs） as stationary phases for capillary gas chromatography （CGC） and to the best of our knowledge,no related reports are available up to now.In this study,a hexaalkylguanidinium ionic liquid（DOTMG-NTf;） was synthesized and coated statically onto capillary columns.Selectivity of the stationary phase was evaluated by separating Grob test mixture,test mixture,alcohols mixture,and fatty acid methyl esters mixture,and thermal stability was investigated as well.The present study demonstrates that GBILs as CGC stationary phases exhibit satisfactory selectivity and thermal stability and have a great potential as new candidates for CGC stationary phases.

Retention behaviors of novel ionic liquid stationary phases and their selectivity for capillary gas chromatography

One chloride-terminated ionic liquid（CTIL） and two hydroxyl-terminated ionic liquids（HTILs） were synthesized and used as stationary phases for capillary gas chromatography（CGC）.Molecular interactions of these stationary phases were evaluated by Abraham solvation parameter model,indicating that the CTIL exhibits remarkably strong H-bond basicity and the HTILs possess both H-bond basicity and acidity.The molecular interactions were further confirmed by separation of a complex mixture consisting of ketones,aldehydes,esters,alcohols and aromatic compounds.It was found that the obtained solvation parameters correlate well with the chromatographic performances of the analytes in terms of elution order and resolution.The well correlated relationship between the solvation parameters and the selectivity of the CTIL and HTILs stationary phases is quite helpful in predicting and understanding the retention behaviors of different types of analytes on these stationary phases.

Selectivity of guanidinium ionic liquid for capillary gas chromatography

A guanidinium ionic liquid,N,N,N＇,N＇-tetrahexyl-N＂,N＂-dimethylguanidinium bis（trifluoromethane）sulfonylimide（THDMGNTf2）, was synthesized and used as stationary phase for capillary gas chromatography.In comparison with imidazolium ionic liquid stationary phase,the present new stationary phase exhibits quite different selectivity and behaves more like a low polar stationary phase.The guanidinium ionic liquid of THDMG-NTf2 exhibited better separation of Grab test mixture than imidazolium ionic liquid of 1-octyl-3-butylimidazolium bis（trifluoromethane）sulfonylimide（OBIM-NTf2）.Solvation parameter model was also used to evaluate the selectivity of THDMG-NTf2.Additionally,essential oil of Magnolia biondii Pamp was analyzed to further evaluate the selectivity of THDMG-NTf2 for a sample of complicated components.Satisfactory separation of the essential oil was achieved on a THDMG-NTf2 column（10 m） while using a commercial column（30 m） as reference.The present study shows that the guanidinium ionic liquid possesses novel chromatographic selectivity and has great potential for wide applications.

Determination Enantiomer Excess(e.e.%)of Chiral Sharpless Epoxides with β-Cyclodextrin Derivatives as Chiral Stationary Phases of Capillary Gas Chromatography

Using four β-cyclodextrin derivatives, 2,6-di-O-benzyl-3-O-heptanonyl-β-CD, 2,6-di- O-benzyl-3-O-octanonyl-β-CD, 2,3-di-O-benzyl-6-O-heptanonyl-β-CD, and 2,3-di-O-benzyl -6-O- octanonyl-β-CD, as chiral stationary phases of capillary gas chromatography （CGC）, the enantiomers of Sharpless epoxides were well separated. The enantiomer excess values （e.e.%） of some chiral Sharpless epoxides were also determined successfully using these CDs.

SIMULTANEOUS DETERMINATION OF EPHEDRINE AND ITS ANALOGUES IN URINE BY CAPILLARY GAS CHROMATOGRAPHY

A method is developed for the simultaneous determination of ephedrine,pseudoephedrine, norephedrine, norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylamine is used as the internal standard.Calibration graphs are linear down to 1.30ug/ml urine.

A NOVEL DERIVATIVE OF β-CYCLODEXTRIN AS CHIRAL SIATIONARY PHASE IN CAPILLARY GAS CHROMATOGRAPHY

A novel β-cyclodextrin derivative, 2, 6-di-O-butyl-3-O-acetyl-β-cyclodex- trin, was prepared and used as chiral stationary phase for capillary gas chromato- graphic resolution of enantiomers, lhe glass capillary columns with the derivative having low melting point and high thermal stability could produce more than 3000 plates per column meter and have proven to be good chlral columns to separate the enantiomers of some amino acids, derivatives of epoxy ethane and alkyl halide, etc.

ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs.

Polysiloxane with Pendant [60]Fulleropyrrolidines as Stationary Phase for Capillary Gas Chromatography

Polysiloxane with pendant [60] fulleropyrrolidines was synthesized and used as the stationary phase for capillary gas chromatography for the first time. A preliminary investigation of its property shows that it has an excellent thermostability and a wide range of allowable operating temperature from 80 degrees C to 360 degrees C.

CAPILLARY GAS CHROMATOGRAPHIC ANALYSES OF THE PETROLEUM HYDROCARBONS IN COASTAL SEAWATER

This study of the petroleum hydrocarbons in coastal seawater, using dichloromethane extraction withO-terphenyl and n-C20 as internal standards, and gas chromatography with silica-capillary-column showedthat the recovery of petroleum hydrocarbons reaches 87.8% and that the lowest detection limit is 0.96μg.This method is reproducible, highly accurate, and applicable for determining the petroleum hydrocarbonsin coastal seawater.

The Enantiomer Separations of Allethrone and Propargyllone Using Two Long Chain Acylated b-Cyclodextrin Derivatives as CGC Capillary Stationary Phases

Using two b-cyclodextrin derivatives (CDs) with long chain of acyl groups as chiral stationary phases (CSPs) of capillary gas chromatography (CGC), the enantiomers of racemic allethrone and propargyllone were well resolved after derived with acetyl chloride. The enantiomer excess values (e.e.%) of 1S-allethrone and 1S-propargyllone were also determined successfully using these CDs.

Capillary Column Coated with Heptakis(2,3, 6-tri-O-octyl)-β-cyclodextrin Using Sol-gel Technology

Heptakis(2, 3, 6-tri-O-octyl)-β-cyclodextrin was coated onto the fused silica capillary by sol-gel technology. Column efficiency and column selectivity were studied. The results indicated that high ability of separation was acquired . Positional isomers of aromatic compounds were well separated.

Determination of Camylofin Dihydrochloride and Nimesulide in Pharmaceutical Preparation by Gas Chromatography

This research paper describes simple analytical method for determination of Camylofin dihydrochloride and Nimesulide in tablet formulation by Gas chromatography method. Benzoic acid was used as internal standard. Validation was carried out in compliance with the International Conference on Harmonization guidelines. The method utilized GC (Agilent Technologies 6890 N Network GC system with FID detector), and RTX-5 capillary column (5% diphenyl-95% dimethyl polysiloxane), 30 m × 0.53 mm, 1.5 μm as stationary phase. Helium was used as the carrier gas at a flow rate of 1.5 mL?min–1. The proposed method was validated for linearity, LOD, LOQ, accuracy, precision, ruggedness and solution stability. It can be conveniently adopted for routine quality control analysis.

微波加工和蒸制杭白菊挥发油成分的GC-MS分析

目的:分析我国浙江省国家杭白菊GAP基地微波加工杭白菊和蒸制杭白菊的挥发油成分,为其质量评价提供科学依据。方法:采用水蒸气蒸馏法提取两种炮制品杭白菊挥发油,用GC毛细管色谱柱进行分析,归一化法测定其相对含量,GC-MS鉴定化学成分。结果:从微波加工杭白菊挥发油中检出119个色谱峰,鉴定了50个化合物,占总挥发油量的67.89%;从蒸制杭白菊挥发油中检出175个色谱峰,鉴定了55个化合物,占总挥发油量的63.64%。结论:微波加工杭白菊挥发油收率为0.40%,蒸制杭白菊挥发油收率为0.19%,两者相差近2.1倍;两者挥发油组成基本相同,唯各化合物含量有一定差异。采用微波干燥技术加工杭白菊,可尽量多地保留了原形挥发油化学成分;与传统的蒸制加工方法比较,大大改善了菊花的等级和质量。

独活挥发油成分的GC-MS分析

目的:分析我国中药材GAP基地之一所种植独活挥发油的化学成分,为其质量评价提供科学依据。方法:采用水蒸气蒸馏法提取独活挥发油,用GC毛细管柱进行分析,归一化法测定其相对含量,并用GC-MS法鉴定化学成分。结果:检出229个色谱峰,鉴定出88个化合物,占挥发油总量的78.23%。结论:独活挥发油的单萜类化合物及其衍生物中,3-蒈烯(8.89%)、间-聚伞花素(4.99%)、β-水芹烯(8.35%)等是主要成分,占总挥发油量的22.23%;倍半萜类化合物及其衍生物中,桉叶烷-4(14),11-二烯(4.36%)、α-芹子烯(1.36%)、喇叭醇(1.14%)、α-甜没药萜醇(6.03%)和1,8-二甲基-4-异丙基-螺环[4.5]+-8-烯-7-酮(4.37%)等是主要成分,占总挥发油量的17.26%。

小亳菊及其硫磺熏制品挥发油成分的GC-MS分析

目的:分析通风晾干品和硫磺熏制品小亳菊的挥发油成分,为其质量评价提供科学依据。方法:采用水蒸气蒸馏法提取2种小亳菊挥发油,用GC毛细管色谱柱进行分析,归一化法测定其相对含量,GC-MS鉴定化学成分。结果:从通风晾干品小亳菊挥发油中检出216个色谱峰,鉴定了50个化合物,占挥发油总量的73.21%;从硫磺熏制品小亳菊挥发油中检出211个色谱峰,鉴定了65个化合物,占挥发油总量的82.32%。结论:通风干燥晾干品小亳菊挥发油收率为3.50%,硫磺熏制品小亳菊挥发油收率为4.22%,两者相差近1.2倍;两者挥发油组成皆以单萜类化合物为特征性成分,倍半萜类化合物为次要成分,但所含化合物有很大的差异。菊花的硫磺熏制加工过程应严格控制和规范化。

商品肉豆蔻挥发油成分的GC-MS分析

目的 :分析商品肉豆蔻挥发油的化学成分 ,为其质量评价提供科学依据。方法 :采用水蒸气蒸馏法提取肉豆蔻挥发油 ,用GC毛细管柱进行分析 ,归一化法测定其相对含量 ,并用GC MS法鉴定化学成分。结果 :分别检出 95～ 118个成分 ,鉴定出 79个化合物 ,占挥发油总量的 95 .18%～ 98.70 %。结论 :肉豆蔻醚 ( 39.6 3% )

桂枝挥发油化学成分的GC/MS分析

目的 :用气相色谱 -质谱法对桂枝挥发油进行化学成分的分析。方法 :采用水蒸气蒸馏法从桂枝中提取挥发油。试用不同类型的毛细管柱进行分析 ,找出最佳分析条件 ,用归一化法测定其百分含量 ,并用气相色谱-质谱法对化学成分进行鉴定。色谱条件 :SE - 5 4毛细管柱 (2 5m× 0 2 5mm ,0 2 5 μm) ,柱温 90℃ (8min)4℃·min-12 30℃ (10min) ;分流进样 ,分流比 1∶5 0 ;进样温度 2 5 0℃ ,FID检测器 ,温度为 2 5 0℃。结果 :共鉴定了 37个成分 ,占挥发油总成分的 92 %以上。结论 :本方法稳定可靠 ,重现性好 。

红心大白菊挥发油成分的GC-MS分析

目的 :分析我国中药材GAP基地红心大白菊挥发油的化学成分 ,为其质量评价提供科学依据。方法 :采用水蒸气蒸馏法提取红心大白菊挥发油 ,用GC毛细管柱进行分析 ,归一化法测定其相对含量 ,并用GC MS法鉴定化学成分。结果 :检出 136个色谱峰 ,鉴定出 4 7个化合物 ,占挥发油总量的 6 2 .2 4 %。结论 :红心大白菊挥发油中 ,雪松醇、喇叭醇和 1 (1,5 二甲基 4 己烯基 ) 4 甲基苯是其主要成分 ,以倍半萜类化合物喇叭醇含量最高 ,占总挥发油量的 13.9%。

GC-MS法测定紫穗槐果实挥发油中的化学成分

目的:采用GC-MS对紫穗槐果实中挥发油成分进行分析。方法:用挥发油提取器对紫穗槐果实中的挥发油进行了提取和测定。采用30m×0.25mm弹性石英毛细管柱,FID检测器,结合GC-MS,对挥发油进行了分析。结果及结论:紫穗槐果实挥发油含量是2.1%,从中分离出30个化合物,鉴定了其中的26个成分,并测定了相对含量,其主要成分为大牦牛儿烯(11.40%)、β-蒎烯(5.85%)、蒈烯-3(3.02%)、古巴烯(5.84%)、石竹烯(8.40%)、奥(4.49%)、D-伪-α雪松烯(4.53%)、1,3,3-三甲基-[2.2.1.02,6]三环已烷(13.63%)。

宽叶羌活根茎和根的挥发油成分的GC-MS分析(英文)

目的分析宽叶羌活(Notopterygium forbesiiBoiss.)根茎和根的挥发油化学成分,为其质量评价提供科学依据。方法采用水蒸气蒸馏法提取宽叶羌活根茎和根的挥发油,用GC毛细管柱进行分析,归一化法测定其相对含量,并用GC-MS法鉴定化学成分。结果共检出217个色谱峰,初步鉴定出100个化合物,占挥发油总量的78·30%。结论宽叶羌活根茎和根的挥发油中的化学成分主要为单萜和倍半萜类化合物,两者分别占总挥发油中化学成分的41·30%和32·65%。这与狭叶羌活根茎和根的挥发油中单萜和倍半萜类化合物分别占总挥发油中化学成分的13·63%和67·93%不同。(1R)-α-蒎烯(3·98 %)、桧烯(2·51 %)、(1S)-β-蒎烯(5·78 %)、m-月桂烯(4·05 %)、柠檬烯(3·55 %)、3,7-二甲基-1,3,7-庚三烯(3·98 %)、γ-萜品烯(8·70 %)、茴香醚(1·78 %)和(1S)-桥环醋酸冰片酯(2·62 %)为单萜类化合物及其衍生物中的主要成分;( +)-β-榄香烯(1·17 %)、异愈创木烯(1·40 %)、( +)-β-没药烯(1·21 %)、(±)-榄香醇(1·42 %)、愈创木醇(1·14 %)、去羟基异菖蒲二醇(1·13 %)、( -)-土青木香烯(1·99 %)、异愈创木醇(9·48 %)、γ-桉醇(1·77 %)、愈创木-1(10)-烯-11-醇(1·12 %)和α-没药醇(5·35 %)为倍半萜类化合物及其衍生物中的主要成分。