互叶白千层挥发性成分的提取和分析

采用水蒸气蒸馏法从互叶白千层叶及嫩枝中提取挥发油中的油相成分,用乙醚作为溶剂从蒸馏残液中萃取挥发油的水溶性物质,利用气相色谱-质谱（GC-MS）联用分析二者的化学成分并进行比较。互叶白千层挥发性成分的油相部分经鉴定确认了27种成分,占油相部分总量的98.60%,主要成分为松油烯-4-醇（52.15%）、γ-松油烯（19.60%）、α-松油烯（5.86%）、α-松油醇（3.93%）、对伞花烃（3.52%）、1,8-桉叶油素（2.67%）;水溶性部分经鉴定确认了61种成分,占水溶性部分总量的79.15%,主要成分为松油烯-4-醇（27.42%）、α-松油醇（6.55%）、香芹酚（5.00%）、1,8-桉叶油素（4.10%）。     

顶空固相微萃取-气相色谱法测定啤酒挥发性风味成分

运用Plackett-Burman法确定了影响顶空固相微萃取法(HS-SPME)萃取啤酒风味成分效率的显著因素,利用Box-Behnken法设计试验得出回归方程,通过Minitab 15软件进行响应面分析得到最优萃取条件:15mL搅拌的样品瓶中加7mL萃取液并添加0.287g/mL氯化钠,在48.90℃环境下萃取45.12min。在此最优萃取条件下,乙醛、二甲基硫醚、乙酸乙酯、乙酸异丁酯、正丙醇、异丁醇、乙酸异戊酯、异戊醇、己酸乙酯和辛酸乙酯的回收率为91.20%~103.46%,标准偏差为1.74%~8.90%。顶空固相微萃取-气相色谱法能准确地分析啤酒的挥发性风味成分。     

Determination of volatile components in cut tobacco with gas chromatography-mass spectrometry and chemometric resolution

Chromatography-mass spectrometry(GC-MS)was used to analyze the volatile components of cut tobacco samples with the help of heuristic evolving latent projections(HELP).After extracting with simultaneous distillation and extraction method,the volatile components in cut tobacco were detected by GC-MS.Then the obtained original two-dimensional data were resolved into pure mass spectra and chromatograms.The qualitative analysis was performed by similarity searches in the national institute of standards and technology(NIST)mass database with the obtained pure mass spectrum of each component and the quantitative results were obtained by calculating the volume of total two-way response.The accuracy of qualitative and quantitative results were greatly improved by using the two-dimensional comprehensive information of chromatograms and mass spectra.107 of 141 separated constituents in the total ion chromatogram of the volatile components were identified and quantified,accounting for about 88.01% of the total content.The result proves that the developed method is powerful for the analysis of complex cut tobacco samples.     

加速溶剂萃取/气相色谱-质谱法分析朝鲜淫羊藿挥发油成分

为探究朝鲜淫羊藿挥发油的化学成分,采用加速溶剂萃取法（ASE）提取朝鲜淫羊藿挥发油,气相色谱-质谱联用（GC/MS）分析检测,在完全随机设计优化ASE的萃取条件下,萃取收率4.0%,通过NIST98谱图库检索,确认挥发油中包含91种化合物,并用峰面积归一化法,求得各化学成分在挥发油中的质量分数.结果表明：朝鲜淫羊藿挥发...     

超声波辐射-异丙醇抽提提取艾叶挥发油

本文采用异丙醇抽提结合水蒸气蒸馏技术提取艾叶中的挥发性组分,经气相色谱-质谱联机分析结果表明：采用该提取工艺获得了丁酸、邻-二甲苯、正丁醚、反式-1-丁氧基-1-丁烯、丁酸-1-甲丙酯等新的挥发油组分。     

不同方法提取樟树落叶挥发油的比较

采用水蒸气蒸馏法（HD）、微波辅助-水蒸气蒸馏法（MAHD）和微波无溶剂提取法（SFME）提取樟树落叶挥发油,用气相色谱-质谱及峰面积归一化法对挥发油成分进行分析鉴定.实验结果表明,3种方法提取的挥发油提取率接近,水蒸气蒸馏法为0.98％,微波辅助-水蒸气蒸馏法为1.12％,微波无溶剂提取法则为1.04％.3种方法提取的挥发油共鉴定出29种化合物,单萜类氧化物和倍半萜氧化物为挥发油的主要成分;HD所得挥发油中香樟醇、桉树叶醇、樟脑和α-松油醇的质量分数分别为25.58％、21.26％、16.79％和11.19％,MAHD为26.29％、28.72％、15.64％和10.16％,SFM为17.74％、17.74％、17.74％和12.46％.不同方法提取的樟树落叶挥发油提取率及成分总体相近,但也存在一定差异,这为进一步开发利用樟树落叶提供了一定的实验依据.     

以气质联用技术对白补药中挥发性成分的分析

为了寻找白补药的应用基础,确定白补药中挥发性物质的主要成分,用气相色谱-质谱联用技术对白补药石油醚浸膏的化学成分进行研究.用75%的乙醇提取白补药,将所得浸膏加水稀释后用石油醚萃取,再用气相色谱-质谱联用技术对石油醚浸膏进行分析,共分离出53个峰.通过中文数据系统检索和质谱资料核对,鉴定出其中46个化合物,其中主要成分为棕榈油酸甲基酯(质量分数28.94%)、硬脂酸甲酯(质量分数6.47%)、3,4,5,6-四甲基-2,5-辛二烯(质量分数5.42%)、6,10,14-三甲基-2-十五烷酮(质量分数5.07%)等.通过鉴定明确了白补药中石油醚部分的主要成分,为该植物的开发利用提供了科学依据.     

Active set truncated-Newton algorithm for simultaneous optimization of distillation column

An active set truncated-Newton algorithm (ASTNA) is proposed to solve the large-scale bound constrained sub-problems. The global convergence of the algorithm is obtained and two groups of numerical experiments are made for the various large-scale problems of varying size. The comparison results between ASTNA and the subspace limited memory quasi-Newton algorithm and between the modified augmented Lagrange multiplier methods combined with ASTNA and the modified barrier function method show the stability and effectiveness of ASTNA for simultaneous optimization of distillation column.     

葵花籽焙烤前后瓜子仁中脂溶性风味物质的研究

用索氏脂肪提取器萃取出普葵原料和其焙烤后瓜子仁中的脂溶性风味物质,用气相色谱-质谱联用法分析其中的化学成分,共检索出39种化学物质,对生熟瓜子仁中主要化学成分进行对比.结果表明：焙烤后瓜子脂溶性风味物质中有2种成分含量比原料增加100倍以上,7种成分含量提高10倍以上,3种成分含量提高5倍以上,7种成分含量提高1到4倍不等,其他成分均有不同程度提高,仅一种成分含量较原料低.     

Fe3O4磁性石墨烯分散固相萃取水中的有机氯污染物

开发负载胶束的磁性Fe₃O₄纳米微粒修饰的石墨烯作为新型分散固相萃取材料,并用于水中有机氯的检测。磁性石墨烯由氧化石墨烯和Fe²⁺通过氧化还原法一步合成,负载阳离子表面活性剂CTAB形成纳米混合胶束作为提取系统。应用本方法分析水中的29种有机氯,检测限达到1.5~5.0 ng/L,样品加标回收率范围在75.22%~97.15%。复重性的相对标准偏差小于9.995%,与传统的固相萃取法相比,方法的灵敏度提高了50~113倍。该方法快速、灵敏、准确,可以同时测定水中多种有机氯农残,适合于大批量样品的测定。     

热脱附、固相微萃取、同时蒸馏萃取对牛肉香精呈香组分提取效果的比较研究

采用热脱附、固相微萃取、同时蒸馏萃取三种不同前处理方法对牛肉香精挥发性风味成分进行提取,利用气质联用仪分析,比较3种方法对提取物种类及提取量的差别.结果显示,3种方法对提取组分的选择性各不相同,如需全面了解样品的香气构成且实验时间允许,应以多种方法综合使用,相互补充.     

Comparative analysis of volatile constituents between herbal pair flos lonicerae-caulis lonicerae and its single herbs

Gas chromatography-mass spectrometry (GC-MS) and the chemometric resolution method (alternative moving window factor analysis, AMWFA) were used for comparative analysis of volatile constituents in herbal pair (HP) flos lonicerae-caulis lonicerae (FL-CL) and its single herbs. The temperature-programmed retention index (PTRI) was also employed for the identification of compounds. In total, 44, 39, and 50 volatile chemical components in volatile oil of FL, CL and HP FL-CL were separately determined qualitatively and quantitatively, accounting for 87.22%, 94.54% and 90.08% total contents of volatile oil of FL, CL and HP FL-CL, respectively. The results show that there are 32 common volatile constituents between HP FL-CL and single herb FL, 33 common volatile constituents between HP FL-CL and single herb CL, and 10 new constituents in the volatile oil of HP FL-CL.     

顶空固相微萃取-气相色谱质谱联用分析汉麻叶挥发性成分

采用顶空固相微萃取法结合气相色谱-质谱联用对汉麻叶的挥发性成分进行分析,考察3种不同萃取纤维（DVB/CAR/PDMS,CAR/PDMS,PDMS/DVB）对分析结果的影响,结果表明较佳萃取纤维为CAR/PDMS.从汉麻叶中检出59种挥发性成分,占挥发油总组分的93.18%,其中醛类3种（0.71%）、醇类1种（0.06%）、烃类37种（57.23%）、杂环化合物类3种（0.19%）、萜烯类12种（34.49%）、其他3种（0.50%）.在鉴定出的成分中含量较多的是[1R-（1R＊,4Z,9S＊）]-4,11,11-三甲基-8-亚甲基-二环[7.2.0]4-十一烯（18.81%）、（1α,3α,5α）-1,5-二甲基-3-甲基-2-亚甲基环己烷（18.18%）、α-石竹烯（11.52%）、异柠檬烯（6.78%）等.     

Organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction

A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS 11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.     

垃圾渗滤液中挥发性有机物的HS-SPME/GC-MS分析

采用顶空固-相微萃取（HS-SPME）和气相色谱-质谱联用仪（GC/MS）检测技术对垃圾渗滤液中挥发性和半挥发性物质进行了分析,所运用的SPME萃取纤维是非键合聚二甲基硅氧烷（以下简称PDMS）,涂层厚度分别为100μm（主要适合挥发性）和7μm（主要适合半挥发性）,在室温下搅拌（1 200 r/min）5 min后,顶空萃取60 min后,迅速在GC-MS进样口250℃解析5 min后进行分析检测.检出挥发性有机物有8种,其中主要类别是酮类、酚类和醇类等3种.     

纳米TiO2／SiO2固相萃取剂的制备及对重金属离子吸附性能的研究

以钛酸四丁酯、正硅酸乙酯作为前驱体,溶胶—凝胶法制备了纳米TiO2／SiO2复合物。采用x射线衍射（XRD）、透射电镜（TEM）、X射线能谱（EDS）等手段对所制得的TiO2／SiO2复合材料进行表征。以纳米TiO2／SiO2复合材料作为填料制成固相萃取小柱,对重金属离子Cu^2＋、Cr^3＋、Pb^2＋和Hg^2＋进行吸附,硝酸洗脱后,采用ICP—MS进行检测。考察了吸附剂对不同pH值溶液中金属离子的吸附性能。自制SPE小柱与ICP—Ms联用测定Cu^2＋、Cr^3＋、pb^2＋和Hg^2＋的最低检出限分别为0．031,0．010,0．041,0．025μg／L。     

Analysis of volatile components in herbal pair herba schizonepetae-ramulus cinnamomi

Analysis of volatile components in herbal pair (HP) herba schizonepetae-ramulus cinnamomi (HS-RC),single herb HS and RC was carried out by gas chromatography-mass spectrometry (GC-MS) data and chemometric resolution method (CRM).The two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound by CRM.In total,47,61 and 51 chemical components in volatile oil of HS,RC,and HP HS-RC were respectively determined qualitatively and quantitatively,accounting for 90.52%,88.37%,and 88.72% total contents of volatile oil of HS,RC,and HP HS-RC,respectively.The number of the volatile components of HP HS-RC is almost the addition of that of two single herbs,but their relative contents are changed.     

在线萃取FIA－GFAAS法测定超痕量金

通过研究在线液－液萃取ＦＩＡ－ＧＦＡＡＳ法测定环境样品中超痕量金的方法，着重探讨了重力分相器的应用前景及其限定条件。在线萃取测定中，Ａｇ的检出限为０．０３ｎｇ／ｍｌ，１ｕｇ／ｍｌＡｕ的测定精度为２．７％（ｎ＝１１），采样频率为３６次／时，富集倍数为２０倍。     

Analysis of volatile chemical components of Radix Paeoniae Rubra by gas chromatography-mass spectrometry and chemometric resolution

The volatile chemical components of Radix Paeoniae Rubra (RPR) were analyzed by gas chromatography-mass spectrometry with the method of heuristic evolving latent projections and overall volume integration. The results show that 38 volatile chemical components of RPR are determined, accounting for 95.21% of total contents of volatile chemical components of RPR. The main volatile chemical components of RPR are (Z, Z)-9,12-octadecadienoic acid, n-hexadecanoic acid, 2-hydroxy- benzaldehyde, 1-(2-hydroxy-4-methoxyphenyl)-ethanone, 6,6-dimethyl-bicyclo[3.1.1] heptane-2-methanol, 4,7-dimethyl-benzofuran, 4-(1-methylethenyl)-1-cyclohexene-1-carboxaldehyde, and cyclohexadecane.     

纺织品中6种禁用有机磷阻燃剂的同时测定

建立了一种同时测定纺织品中6种禁用有机磷阻燃剂的气质联用方法,该方法以丙酮为萃取溶剂,采用微波辅助萃取技术萃取纺织品中的禁用有机磷阻燃剂,萃取液进行气相色谱/质谱-选择离子监测测定.6种目标分析物的检出限为1 ng/mL～1μg/mL,方法的加标回收率为84.99%～94.87%,相对标准偏差为4.04%～9.37%.该方法灵敏度高、操作简便快速、定性定量准确.采用该方法对市售的阻燃纺织品进行测定,结果发现部分样品中含有高浓度的禁用有机磷阻燃剂.