固相微萃取-气相色谱-质谱联用分析白苏子挥发性化学成分

目的分析白苏子中挥发性成分的组成,为其开发利用提供科学依据。方法采用固相微萃取（SPME）法萃取白苏子中的挥发性物质,并用气相色谱-质谱（GC-MS）法对其挥发性化学成分进行分析。结果共分离出60个色谱峰,并且确定了其中47个成分,占挥发性成分总量的89.73%。其中主要化学成分是羊脂酸（8.94%）,正己醛（8.31%）,天竺葵醛（6.27%）,（E,E）-3,5-辛二烯-2-酮（5.19%）。结论白苏子中含有丰富的挥发性成分,SPME-GC-MS联用能全面快速获得其组成信息,可应用于白苏子挥发性成分的分析。     

固相微萃取技术/气相色谱/质谱分析水菖蒲挥发性化学成分

目的:分析水菖蒲挥发性化学成分。方法:利用固相微萃取/气相色谱/质谱(SPME/GC/MS)联用技术对水菖蒲挥发性成分进行研究。结果:共鉴定出69种化学成分,占挥发性总成分的81.75%。结论:水菖蒲主要挥发性化学成分是1,4-顺-1,7-顺-菖蒲烯酮(11.72%),2-β-异丙烯基-6-α-异丙烯基-3-β-甲基-3-α-乙烯基环己酮(6.04%),β-倍半水芹烯(5.71%),α-佛手柑油烯(4.58%),γ-紫穗槐烯(4.11%),γ-杜松烯(4.07%),顺-甲基-异丁香油酚(4.03%)等。     

固相微萃取-气相色谱-质谱联用分析贵州产杏叶茴芹挥发性成分

目的:研究贵州产杏叶茴芹挥发性成分。方法:采用固相微萃取技术对杏叶茴芹挥发性成分进行提取,GC-MS进行鉴定。结果:从杏叶茴芹挥发性成分中得到28个组分,鉴定了其中的19个化合物,占挥发性成分的86.23%。主要挥发性成分为(S)-1-甲基-4-(5-甲基-1-甲基-4-己烯基)环己烯(48.83%)和1-(1,5-二甲基-4-己烯基)-4-甲基苯(6.15%)。结论:杏叶茴芹挥发性成分主要是萜烯类。     

西府海棠挥发性成分研究

目的分析西府海棠花的挥发性成分。方法采用顶空固相微萃取和气质联用技术（HS-SPME-GC-MS）进行分析。结果从西府海棠花中鉴定了47种组分,用峰面积归一化法测定,其相对含量占总挥发性组分峰面积的91.71%。结论首次分析了西府海棠花的挥发性成分,指出西府海棠花的潜在药用价值和赋香成分,为进一步开发利用西府海棠资源提供了依据。     

顶空固相微萃取-气质联用法分析新鲜假蒟挥发性化学成分

目的:研究新鲜假蒟的挥发性化学成分.方法:采用顶空固相微萃取-气质联用技术(HS-SPME-GC-MS).结果:共鉴定出48种化合物,按峰面积比占假蒟挥发油化学成分的88.7％,其中β-月桂烯(34.4％)、α-水芹烯(5.5％)、柠檬烯(8.9％)、芳樟醇(6.0％)为主要化合物.结论:方法具有简便、快速、准确、样品量小等特点,适用于新鲜假蒟挥发性化学成分的快速测定.     

HS-SPME-GC/MS分析鸡矢藤挥发性成分

目的:分析鸡矢藤的挥发性成分。方法:采用顶空固相微萃取和气质联用技术(HS-SPME-GC/MS),结合保留指数法并用峰面积归一化法测定相对含量。结果:从鸡矢藤中鉴定出了18个挥发性成分,占总峰面积的95.28%,其中百里香酚(30.97%),二甲基二硫(9.78%),喹啉(5.74%),十六酸(5.53%),邻苯二甲酸二丁酯(5.07%),邻苯二甲酸二甲酯(3.67%),壬醛(3.65%)和邻苯二甲酸二异丁酯(3.18%)等的含量较高。结论:鸡矢藤的主要挥发性成分为百里香酚和邻苯二甲酸酯类。     

PBTK modelling platforms and parameter estimation tools to enable animal-free risk assessment: Recommendations from a joint EPAA – EURL ECVAM ADME workshop

Information on toxicokinetics is critical for animal-free human risk assessment. Human external exposure must be translated into human tissue doses and compared with in vitro actual cell exposure associated to effects (in vitro–in vivo comparison). Data on absorption, distribution, metabolism and excretion in humans (ADME) could be generated using in vitro and QSAR tools. Physiologically-based toxicokinetic (PBTK) computer modelling could serve to integrate disparate in vitro and in silico findings.     

顶空固相微萃取-气质联用法测定热加工食品中的呋喃

目的:建立顶空固相微萃取(HS-SPME)结合气相色谱质谱(GC/MS)测定热加工食品中呋喃的方法。方法:试样中加入d4-呋喃内标和2 g氯化钠,采用75μm CAR/PDMS萃取头,25℃下萃取30 min后,在气相色谱质谱仪进样口280℃解吸2 min,PLOT Q毛细管柱气相色谱分离,选择离子监测(SIM)模式定量测定。结果:方法线性范围为1 ng/g～50 ng/g,方法检出限(S/N≥3)为0.2 ng/g,定量检出限(S/N≥10)为1.0 ng/g;不同基底样品中加标回收率为87.8%～92.5%,相对标准偏差值(RSD)为1.2%～3.1%。结论:该方法灵敏度高、准确可靠,可分析热加工食品中呋喃的含量。     

Microwave assisted solid phase microextraction for extraction and selective enrichment of four alkaloids in lotus leaf

A novel method was developed for extraction and enrichment of the four alkaloids (nuciferine, O-nornuciferine, armepavine and N-nornuciferine) from lotus leaf by coupling microwave-assisted extraction (MAE) with solid phase microextraction (SPME) before ultra-high-performance liquid chromatography (UHPLC) analysis. The influence parameters of MAE and SPME process including solvent-to-materials ratio, extraction solvent, irradiation power, extraction time were investigated. The method exhibited a good linearity within the range of 0.4–100 μg mL^?1 for nuciferine and O-nornuciferine, 0.1–25 μg mL^?1 for armepavine and N-nornuciferine (r² > 0.9990), respectively. Compared with the other extraction method, this method obviously shortens analytical time and enhances extraction efficiency. In addition, the concentration of the four alkaloids (nuciferine, O-nornuciferine, N-nornuciferine and armepavine) included two trace alkaloids were increased by 13, 10, 5 and 12 times after concentration, respectively. It was concluded that the newly MAE-SPME was an efficient method for the extraction and enrichment for alkaloids from herbs.     

In-matrix derivatization and automated headspace solid-phase microextraction for GC-MS determination of amphetamine-related drugs in human hair

A fully automated method for analysis of amphetamine-related drugs in human hair by gas chromatography-mass spectrometry (GC-MS) was developed using headspace solid-phase microextraction (SPME) and in-matrix derivatization. Amphetamines were extracted from hair under alkaline conditions, and were simultaneously derivatized to N-ethoxycarbonyl amphetamines with ethylchloroformate in a vial. An SPME fiber was then exposed to the headspace at 80°C for 10 min for extraction. The derivatives extracted into the stationary phase of the fiber were desorbed by exposing the fiber in an injection port of a GC-MS instrument. The calibration curves showed linearity up to 10ng/mg in hair. The detection limits ranged from 0.01 to 0.5 ng/mg according to the compound identity. No interferences were found, and the time required for analysis was about 30 min per sample. Furthermore, this proposed method was applied to diagnosis of methamphetamine intake in actual cases; methamphetamine and its metabolite amphetamine were able to be detected in hair of abuser patients admitted to a hospital.