气相色谱-质谱测定红树植物桐花树叶中的挥发油和脂肪酸的组成

采用气相色谱-质谱联用分析法,分析测定了红树植物桐花树AegicerasCorniculatum叶子中挥发油和脂肪酸的成分.结果表明:挥发油中分离出24个峰,鉴定出8种化合物,2,6-二叔丁基-4-甲基苯酚含量丰富,占挥发油总量的20.60%;脂肪酸中分离出16个峰,鉴定出10种脂肪酸,其中主要成分有十六酸(棕榈酸,16.17%)、9,12-十八碳二烯酸(亚油酸,25.73%)、9-十八碳烯酸(油酸,41.52%)等.     

气相色谱-质谱法分析木奶果挥发油的化学成分

采用水蒸汽蒸馏法从大戟科木奶果中提取挥发油,用气相色谱-质谱对挥发油的化学成分进行了分析。鉴定出19种化合物,占总油量的100%,用面积归一化法测定了各成分的相对百分含量。木奶果挥发油主要成分为正十六碳酸、丁基甲氧基苯、9,12-十八碳二烯酸,分别占挥发油总量的29.53%、17.47%和11.59%,三者占其总量的58.59%。     

气相色谱-质谱联用法测定槐花中挥发性化学成分

槐花样品经蒸气蒸馏及乙醚萃取处理所得挥发油,用气相色谱-质谱联用法进行分析,按峰面积归一化法求出挥发性化学成分的相对含量.分离出42个峰,已鉴定了26个化合物,占其挥发油总相对含量的87.76%.已鉴定的有酸、酯、烯烃、醇、烷烃等10类化合物.其中酸类化合物占总色谱流出峰面积的30.53%,酯类占19.26%,烯烃类占18.01%,醇类占8.64%,烷烃类占5.52%.其主要组分有n-十六酸(26.43%)、17-三十五(烷)烯(14.84%)、喇叭茶萜醇(8.00%)、十六酸甲酯(4.18%)、肉豆蔻酸(4.10%)、8,11-十八碳二烯酸甲酯(3.79%)、月桂酸酐(3.60%)、9-十八(碳)炔酸甲酯(3.26%)、1,2-邻苯二甲酸丁基环己基酯(3.03%)、c-榄香烯(2.66%).     

鸢尾根挥发性成分的GC-MS分析

采用气相色谱-质谱联用技术对罗布麻的挥发性成分进行了分离鉴定.分离出40种成分,共确认了其中26种成分,占挥发油总含量的86.6%.采用峰面积归一化法确定了各成分的相对含量,其中主要成分为3-甲氧基-1,2-丙二醇(29.54%)、月桂酸(12.04%),癸酸(4.52%)、9,12-十八碳二烯酸甲酯(4.15%)、棕榈酸(3.91%)、月桂酸乙酯(3.87%)、庚烷(3.74%)、肉豆蔻酸(3.69%).     

气相色谱-质谱联用法测定印度楝树油中高级脂肪酸组分含量

对印度楝树油中高级脂肪酸成分进行分析,经甲酯化后用气相色谱-质谱联用仪鉴定了 其中所含高级脂肪酸的成分,用气相色谱法-火焰离子化检测器对其成分进行定量分析.溶剂浸泡萃取和二氧化碳超临界萃取两种不同方法得到的脂肪酸成分基本相同,其中油酸相对含量为51.15%,硬脂酸相对含量为19.13%,棕榈酸相对含量为16.78%,亚油酸相对含量为9.86%,花生酸相对含量为1.24%,其他含量低于1%的高级脂肪酸还有顺-3-辛基-环氧乙烷-辛酸,山萮酸,9-十八(碳)烯酸,11-二十碳二烯酸,9-十六碳烯酸,十七(烷)酸等.     

鸢尾根挥发性成分的GC-MS分析

采用气相色谱-质谱联用技术对罗布麻的挥发性成分进行了分离鉴定。分离出40种成分,共确认了其中26种成分,占挥发油总含量的86.6%。采用峰面积归一化法确定了各成分的相对含量,其中主要成分为3-甲氧基-1,2-丙二醇(29.54%)、月桂酸(12.04%),癸酸(4.52%)、9,12-十八碳二烯酸甲酯(4.15%)、棕榈酸(3.91%)、月桂酸乙酯(3.87%)、庚烷(3.74%)、肉豆蔻酸(3.69%)。     

用GC-MS法观察3个不同产地山茱萸的挥发油成分

采用气相色谱-质谱法(GC-MS)研究3个不同产地山茱萸果肉的挥发油成分.结果发现主要成分有差异,河南和山西产山茱萸挥发油的主要成分有棕榈酸(1 2.6 0、1 7.1 7)、十八碳二烯酸(1 0.2 8、3.9 4)、十八碳三烯酸(1 4.3 0、6.0 3),而在陕西产山茱萸挥发油中不存在这3种成分;河南和陕西产山茱萸挥发油中有很多酰胺类、酯类化合物;山西产山茱萸挥发油中的特殊成分是1-乙酰基-4,6,8-三甲基甘菊环.3产地山茱萸果肉挥发油中共有成分为1,2,4 a,5,6,8 a-六氢-4,7,-二甲基-1-异丙基萘、a-杜松醇、1,4-二甲基-6-异丙基萘、邻苯二甲酸二异丁酯、7-羟基卡达烯.     

棉籽化学成分的分析

采用索氏提取法对棉籽中棉籽油进行了提取,以气相色谱-质谱联用仪进行了分析,分离鉴定出10种脂肪酸,占棉籽油总量的99.52%。并对其主要成分进行了鉴定,主要化学成分为:棕榈酸26.68%,亚油酸66.05%。用蒸馏-萃取法提取棉花籽中挥发性物质,测得棉籽挥发油的量为0.80%,用GC/MS法从棉籽挥发油中分离并确定出16种化学成分。用峰面积归一化法通过化学工作站数据处理系统,得出各化学成分在挥发油中的质量分数。其中主要成分为:石竹烯量高达33.27%。     

一种氨基哌嗪功能化的丹磺酰氯荧光衍生试剂的合成及其在高效液相色谱法定量分析微藻油脂中的应用北大核心CSCD

自制氨基哌嗪功能化丹磺酰氯(DNS-CL)荧光衍生试剂(DNS-Pi-NH_(2)),并用其衍生化小球藻中碳原子数为10~20的典型脂肪酸[十二烷酸、十四烷酸、顺-9,12-十八(碳)烯酸、顺-7,10,13-十六(碳)烯酸、十六烷酸、顺-9-十八(碳)烯酸、十八烷酸、二十烷酸],用高效液相色谱法(HPLC)测定8种脂肪酸的含量。将小球藻脂肪酸甲酯样品用含氢氧化钾的乙醇溶液于79℃皂化60 min,滴加盐酸溶液,直至酚酞指示剂由红色变为无色。蒸发除去乙醇,所得固体经水清洗、离心、振荡、过滤,即制得小球藻脂肪酸样品。以DNS-CL和N-(2-氨基乙基)哌嗪为原料制备DNS-Pi-NH_(2),并用红外光谱、核磁共振碳谱、质谱对其结构进行表征。取制备好的DNS-Pi-NH_(2)、二丙基二硫醚、三苯基磷的乙腈溶液和1.0 mg小球藻脂肪酸样品在室温下振荡衍生10 min,所得溶液用90%(体积分数,下同)乙腈溶液稀释后,用HPLC测定其中脂肪酸衍生物的含量。以Eclipse XDB C_(8)色谱柱为固定相,以90%乙腈溶液为流动相进行等度洗脱,分离得到的目标物用荧光检测器检测。结果显示:8种脂肪酸衍生物在30 min内可实现完全分离;各脂肪酸的浓度在2.0×10^(-10)~2.0×10^(-4)mol·L^(-1)内与其对应的峰面积呈线性关系,检出限(3s/k)为21~65 pmol·L^(-1);对微藻培养液样品进行加标回收试验,所得回收率为95.3%~102%,测定值的相对标准偏差(n=5)为1.7%~2.6%;方法用于小球藻脂肪酸甲酯样品的分析,检出了十六烷酸、顺-9,12-十八(碳)烯酸、顺-7,10,13-十六(碳)烯酸、顺-9-十八(碳)烯酸,检出量分别为3.08,0.64,0.83,2.57 mg·g^(-1)。     

油松籽油脂的提取及其脂肪酸组成与含量的评价

采用索氏提取法提取油松籽中的油脂,得油率为42.9%;对油脂进行甲酯化处理后用气相色谱-质谱联用仪检测其中的脂肪酸组成及含量。实验结果表明,油松籽油中含有7种脂肪酸,分别为肉豆蔻酸10.38%、硬脂酸3.05%、油酸21.98%、亚油酸(13,16-十八碳二烯酸)3.53%、亚油酸(9,12-十八碳二烯酸)38.38%、亚麻酸20.06%和二十碳三烯酸2.62%,其中饱和脂肪酸含量为13%,不饱和脂肪酸含量为87%。     

肉苁蓉挥发性化学成分分析

报道了用同时蒸馏—萃取法提取肉苁蓉挥发性物质，测得肉苁蓉挥发油的含量为3．5％；利用GC／MS法分离确认出24种化学成分；用峰面积归一化法得出各化学成分在挥发油中的相对百分含量，其中主要成分为丁香酚，占总挥发油的83．60％；又用单离子法分离出丁香酚，并用IR，EI-MS法对其进行分析确认。     

三岛柴胡种子化学成分分析

应用ＧＣ／ＭＳ技术对云南省文山县引种的日本三岛柴胡种子的挥发油和脂肪酸成分进行定性定量分析,检出５３个挥发油成分和２８个脂肪酸成分,挥发油以４,４,５－三甲基－２－乙烯、２,２,４－三甲基－３－戊烯－１－醇、２,３－二甲基丁烯－３－二甲基戊烷为主;脂肪酸以十八碳烯酸,十八烷酸,壬二酸和辛二酸为主。从种子的正丁醇提取部分还分离出８个皂甙,其中３个鉴定为柴胡皂甙ｄ,ｃ和６″－Ｏ－乙酰基柴胡皂甙ｄ。     

黄柏挥发性化学成分分析

报道了用同时蒸馏－萃取装置（SDE）提取黄柏的挥发性物质,测得黄柏挥发油的含量为0．45％,用GC／MS法从黄柏挥发油中分离并确认出41种化学成分;用峰面积归一化法通过化学工作站数据处理系统得出各化学成分在挥发油中的百分含量,其中主要成分为酮类（16．38％）、醛类（13．94％）、醇类（8．27％）、酚类（50．38％）、酸类（2．18％）、其他类成分仅占3．33％,共占总检出量的97．5％。     

气相色谱/质谱法分析曼陀罗果实挥发油的化学成分

用水蒸汽蒸馏法从曼陀罗果实中提取挥发油,并用气相色谱/质谱(GC/MS)联用技术对其化学成分进行分离和结构鉴定,用峰面积归一化法确定各成分的相对含量。结果确定了68种化合物,占挥发油总量的82.83%,其主要成分为6-戊基-5,6-二氢化吡喃-2-酮(9.13%)、3,7,11,15-四甲基-2-十六碳烯-1-醇(6.71%)、二苯酮(6.16%)和1-己醇(6.10%)等。     

Determination of volatile flavor components in danggui cultivars by solvent free injection and hydrodistillation followed by gas chromatographic-mass spectrometric analysis

The rhizome of Angelica gigas Nakai, Angelica sinensis Diels and Angelica acutiloba Kitagawa (Umbelliferae) were chopped and extracted by hydrodistillation (HD) and solvent free solid injector (SFSI) methods to obtain the volatile compounds that were then characterized and identified by gas chromatography-mass spectrometry (GC/MS). SFSI extraction yielded a generally higher amount of volatile compounds than that produced by HD. A total of 48 components [including terpenes (8), aldehydes (4), alcohol (2), coumarins (9), Phthalide (3), acids (2) and sterols (2)] were identified by SFSI and gas chromatography-mass spectrometry from the three species of danggui cultivars, whereas, 24-essential oil was obtained by HD for Korean danggui only. According to these analyses, several coumarin derivatives such as decursinol angelate (16.83%) and decursin (29.34%) were found to be the dominant ones, followed by lomatin (10.25%) and marmesin (9.33%) in Korean danggui. Furfural and butylidene phthalide were the main components in Japanese in addition to butylidene dihydro-phthalide in Chinese danggui. Some parameters affecting the extraction efficiency such as injector temperature, injection time and pre-heating time were optimized. The results showed that the SFSI-method gave a higher yield of components with higher molecular mass than hydrodistillation. SFSI required little time to prepare the sample, little sample mass and a small quantity of organic solvent was needed. It can be concluded that analysis of volatile flavor compounds by SFSI in combination with gas chromatography/mass spectrometry is a suitable monitoring technique to differentiate danggui cultivars.     

Analysis of volatile components from Melipona beecheii geopropolis from Southeast Mexico by headspace solid-phase microextraction

A head space solid-phase microextraction method combined with gas chromatography–mass spectrometry was developed and optimised to extract and analyse volatile compounds of Melipona beecheii geopropolis. Seventy-three constituents were identified using this technique in the sample of geopropolis collected. The main compounds detected include β-fenchene (14.53–15.45%), styrene (8.72–9.98%), benzaldehyde (7.44–7.82%) and the most relevant volatile components presents at high level in the geopropolis were terpenoids (58.17%).     

Analysis of Artemisia annua L. volatile oil by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry

Artemisia annua L. is an annual herb native of Asia, it has been used for many centuries for the treatment of fever and malaria. In this paper, analysis of the volatile oil of Artemisia annua L. was performed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC x GC-TOF MS). Three hundred and three components were tentatively identified and terpene compounds are the main components of Artemisia annua L. volatile oil. Artemisinic acid is tentatively qualified.     

顶空固相微萃取-气相色谱-质谱分析发酵香肠挥发性成分

采用固相微萃取-气相色谱-质谱(SPME-GC-MS)联用分析技术对发酵香肠挥发性成分进行了分析。共鉴定了33种化合物。结果表明，发酵香肠的挥发性成分主要为醇类、酮类、酯类、有机酸类、酚类及醛类等。     

Floral scent composition of Plumeria tuberculata analyzed by HS-SPME

The headspace volatile compounds of the flowers of Plumeria tuberculata Lodd. were analyzed by solid phase microextraction coupled with capillary gas chromatography/mass spectrometry. Twenty-five compounds were identified, representing 100% of the total composition. The volatile fraction was characterized by oxygenated monoterpenes (79.6%), oxygenated sesquiterpenes (8.4%), sesquiterpene hydrocarbons (7.6%), and benzenoid esters (2.6%). The major components were geraniol (34.9%), citronelol (21.5%) and geranial (16.2%), and they were found to make the major contribution to the typical scent of this flower.     

Comprehensive chemical profiling and quantification of Shexiang Xintongning tablets by integrating liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry

Shexiang Xintongning tablet (SXXTN) is a traditional Chinese medicine (TCM) preparation for the treatment of coronary heart disease (CHD) angina pectoris. However, due to the complexity of the compounds in SXXTN, the active chemical components responsible for the therapeutic effect are still ambiguous. The purpose of our study was to characterize the chemical profile of SXXTN and quantify the representative chemicals. The high-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-QTOF MS) method and gas chromatograph coupled with mass spectrometry (GC–MS) method were utilized to identify the chemical constituents of SXXTN. A total of 140 compounds including alkaloids, ginsenosides, organic acids, esters, triterpenes, phthalides and amino acid were identified in accordance with their retention times, accurate masses and characteristic MS/MS fragment patterns. Forty-four volatile components were characterized by GC–MS through NIST database matching. In the further research of quantitative analysis, 40 non-volatile compounds and 17 volatile compounds were determined and successfully applied for detecting in 7 batches of SXXTN samples by high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HPLC-QQQ MS) and gas chromatograph coupled with triple-quadrupole tandem mass spectrometry (GC-QQQ MS) in multiple reaction monitoring (MRM) mode, respectively. The quantitative methods were verified in linearity, precision, repeatability stability and recovery. The above results indicated that the established method was practical and reliable for synthetical quality evaluation of SXXTN. In addition, our study might supplement the chemical evidence for disclosing the material basis of its therapeutic effects.