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微波辅助液液微萃取-气相色谱-质谱分析蔬菜、水果中的多种拟除虫菊酯残留 被引量:45
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作者 郑孝华 《分析化学》 SCIE EI CAS CSCD 北大核心 2004年第2期225-228,共4页
将微波辅助萃取同液液微萃取技术相结合 ,利用气相色谱 质谱分析技术 ,结合时间编程 选择离子检测模式 ,开发了一种简捷、实用、回收率高的蔬菜、水果中多种拟除虫菊酯残留的检测技术。该技术同当前执行的国标方法相比 ,有机溶剂用量... 将微波辅助萃取同液液微萃取技术相结合 ,利用气相色谱 质谱分析技术 ,结合时间编程 选择离子检测模式 ,开发了一种简捷、实用、回收率高的蔬菜、水果中多种拟除虫菊酯残留的检测技术。该技术同当前执行的国标方法相比 ,有机溶剂用量少 ,操作简便 ,提取液无须严格净化便可进行GC/MS分析 ,大大提高了分析速度。经基体标准加入回收实验 ,除联苯菊酯外 ,其他 9种菊酯的 10ng/g的加样回收率均在 75 %以上 ,且在国标要求的最大残留限量附近有良好的线性关系 ,能满足当前蔬菜。 展开更多
关键词 蔬菜 水果 拟除虫菊酯 药物残留 微波萃取 液液微萃取 气相色谱 质谱 杀虫剂
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Volatile profile analysis and quality prediction of Longjing tea(Camellia sinensis) by HS-SPME/GC-MS 被引量:40
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作者 Jie LIN Yi DAI +2 位作者 Ya-nan GUO Hai-rong XU Xiao-chang WANG 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2012年第12期972-980,共9页
This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyze... This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS).Pearson's linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds. Results showed that 60 volatile compound scould be commonly detected in this famous green tea. Terpenes and esters were two major groups characterized,representing 33.89% and 15.53% of the total peak area respectively. Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea, especially linalool (0.701), nonanal (0.738), (Z)-3-hexenyl hexanoate (-0.785), and β-ionone (-0.763). On the basis of these 10 compounds, a model (correlation coefficient of89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjingtea. Summarily, this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MStechnique. 展开更多
关键词 Partial least square (PLS) regression Green tea Headspace solid phase microextraction (HS-SPME) Volatile profile Quality prediction
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Time-dependent categorization of volatile aroma compound formation in stewed Chinese spicy beef using electron nose profile coupled with thermal desorption GC–MS detection 被引量:23
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作者 Hui Gong Zhen Yang +4 位作者 Meng Liu Zhijia Shi Jiapeng Li Wenhua Chen Xiaoling Qiao 《Food Science and Human Wellness》 SCIE 2017年第3期137-146,共10页
In the present study,flavor profiles of Chinese spiced beef in the cooking process were comparatively analyzed by electronic nose,gas chromatography–mass spectrometry(GC–MS)with a thermal desorption system(TDS),and ... In the present study,flavor profiles of Chinese spiced beef in the cooking process were comparatively analyzed by electronic nose,gas chromatography–mass spectrometry(GC–MS)with a thermal desorption system(TDS),and solid-phase microextraction(SPME).A total of 82 volatile compounds were identified,and 3-methyl-butanal,pentanal,hexanal,-xylene,heptanal,limonene,terpinene,octanal,linalool,4-terpinenol,-terpineol,and(E)-anethole were identified as the characteristic flavor compounds in Chinese spiced beef.Variation in the content of volatile components produced by different cooking processes was observed.In general,a cooking time of 4 h resulted in optimal flavor quality and stability.Results indicated that the electronic nose could profile and rapidly distinguish variation among different cooking time.The volatile profiling by TDS-GC–MS and responses from the electronic nose,in combination with multivariate statistical analysis,are a promising tool for control the cooking process of spiced beef. 展开更多
关键词 Beef flavor Gas chromatography-mass spectrometry Electronic nose Thermal desorption system Solid-phase microextraction
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Comparison of Headspace Solid-Phase Microextraction with Simultaneous Steam Distillation Extraction for the Analysis of the Volatile Constituents in Chinese Apricot 被引量:20
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作者 CHEN Mei-xia CHEN Xue-sen +4 位作者 WANG Xin-guo CI Zhi-juan LIU Xiao-li HE Tian-ming ZHANG Li-jie 《Agricultural Sciences in China》 CAS CSCD 2006年第11期879-884,共6页
Volatile constituents in fully mature fruits of apricot (Prunus armeniaca L.) cultivar Xinshiji were extracted using headspace solid-phase microextraction (HS-SPME) and simultaneous steam distillation extraction ... Volatile constituents in fully mature fruits of apricot (Prunus armeniaca L.) cultivar Xinshiji were extracted using headspace solid-phase microextraction (HS-SPME) and simultaneous steam distillation extraction (SSDE) and then analyzed using capillary gas chromatography and gas chromatography-mass spectrometry. A total of 70 components were identified by HSSPME, including 20 esters, 19 hydrocarbons, 5 alcohols, 5 ketones, 4 acids, 4 lactones, 3 aldehydes, and 10 miscellaneous components, with the esters being the dominant constituent. On the basis of the odor unit values, it is believed that the following compounds probably contributed to the fresh apricot odor: hexyl acetate, β-ionone, butyl acetate, (E)-2-hexenal, linalool, limonene, γ-decalactone, and hexanal. A total of 49 components were also detected by SSDE, including 13 hydrocarbons, 9 alcohols, 7 aldehydes, 9 esters, 4 ketones, 4 lactones, 2 acids, and 1 miscellaneous component, of which the monoterpene alcohols were the dominant constituents. It could be judged from the odor unit values that the following compounds were the major contributors to boiled apricot aroma: β-ionone, linalool, hexyl acetate, γ-dodecalactone, γ- decalactone, (E)-2-hexenal, hexanal, γ-octalactone, phenylacetaldehyde, butyl acetate, limonene, α-terpineol, and δ-decalactone. The results show that HS-SPME is a simple, rapid, and solvent-free method, which is an alternative to the classical SSDE. 展开更多
关键词 AROMA volatile constituents APRICOT solid-phase microextraction simultaneous distillation-extraction
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应用顶空-固相微萃取结合气相色谱-质谱联用技术分析传统锦州虾酱中挥发性物质 被引量:19
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作者 李莹 吕欣然 +6 位作者 马欢欢 缪璐欢 杜静芳 白凤翎 徐永霞 季广仁 励建荣 《食品与发酵工业》 CAS CSCD 北大核心 2016年第9期210-216,共7页
传统锦州虾酱是以白虾和乌虾为原料,在高盐条件下经长时间发酵形成海产风味食品。采用HPSPME/GC-MS结合保留指数方法分析虾酱中的挥发性物质,并对萃取条件进行优化。从DVB/PDMS、CAR/PDMS和DVB/CAR/PDMS筛选出最佳萃取头,同时采用正交... 传统锦州虾酱是以白虾和乌虾为原料,在高盐条件下经长时间发酵形成海产风味食品。采用HPSPME/GC-MS结合保留指数方法分析虾酱中的挥发性物质,并对萃取条件进行优化。从DVB/PDMS、CAR/PDMS和DVB/CAR/PDMS筛选出最佳萃取头,同时采用正交试验优化SPME参数条件,确定适宜萃取条件为75μm CAR/PDMS萃取头,样品质量为5.0 g,萃取温度为70℃,萃取时间为50 min。对虾酱的风味物质分析得到44种挥发性物质,分别为醛类、酮类、酯类、酸类、酚类、烷烃类、吡嗪类和其他化合物。其中白虾虾酱主要呈香物质是醛类、吡嗪类和酚类等低阈值化合物,3-甲硫基丙醛、四甲基吡嗪和吲哚可能是白虾虾酱有别于乌虾虾酱的特有风味物质。乌虾虾酱主要呈香物质是醛类、酯类、酸类和酚类等低阈值化合物,酸类化合物是乌虾虾酱有别于白虾虾酱特有的风味物质,酯类化合物也可能是乌虾虾酱中风味物质的增味剂。 展开更多
关键词 传统锦州虾酱 挥发性物质 顶空-固相微萃取(headspace solid-phase microextraction HS-SPME) 气相色谱-质谱联用(gas chromatography-mass spectrometry) 保留指数
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GC-MS, GC-O and OAV analyses of key aroma compounds in Jiaozi Steamed Bread 被引量:20
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作者 Yuanhui Wang Jingwen Zhao +6 位作者 Fei Xu Xiaoyun Wu Wenxuan Hu Yongfeng Chang Lanlan Zhang Jie Chen Changhong Liu 《Grain & Oil Science and Technology》 2020年第1期9-17,共9页
Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS... Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS-SPME).These volatile substances were analyzed by gas chromatography-mass spectrometry(GC-MS)and gas chromatographyolfactometry-mass spectrometry(GC-O-MS).The results demonstrated that 61 volatile compounds were identified totally in samples,of which 15 were confirmed as potent aroma compounds with odor active values(OAVs)>1.The 15 potent aroma compounds were ethanol,1-butanol,1-pentanol,1-hexanol,heptanol,1-octen-3-ol,3-methyl-1-butanol,hexanal,heptanal,nonanal,(E)-2-heptenal,benzaldehyde,(E,E)-2,4-decadienal,2-pentylfuran and naphthalene.The SDEmethod had better linearity with coefficients of determination(R2)equal to or higher than 0.9991.Furthermore,the SDE method also achieved lower sensitivity and better repeatability and recovery than HS-SPME.This work provides reference method and parameters for future research on the flavor of JSB for commercial products. 展开更多
关键词 Volatile compounds Simultaneous distillation and extraction HEADSPACE SOLID-PHASE microextraction Quantitative analysis Method validation
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Study on the Chromatographic Fingerprint of Volatile Constituents from Acacia Honey 被引量:19
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作者 夏立娅 张晓宇 +1 位作者 王庭欣 马英松 《Agricultural Science & Technology》 CAS 2010年第6期42-44,共3页
[Objective] The experiment aimed to study chromatographic fingerprint in volatile components of acacia honey and provide scientific evaluation and effective control on quality of acacia honey.[Method] Using solid-phas... [Objective] The experiment aimed to study chromatographic fingerprint in volatile components of acacia honey and provide scientific evaluation and effective control on quality of acacia honey.[Method] Using solid-phase microextraction method to separate and detect volatile components and construct chromatographic fingerprint.[Result] The honey was preheated for 15 min in water bath at 40 ℃ and solid-phase microextraction 85 μmPA was used to extract in overhead air about 30 min,then put it into the injector and desorpted 3 min,which is in 230 ℃.The Supelco WaxTM10 30 m×0.25 mm×0.25 μm column and gradient heating program was the best method to separate volatile components from honey.83 fingerprint peaks were constructed,among which 17 common fingerprint peaks were comprised of chromatographic fingerprint of volatile components of acacia honey.[Conclusion] The chromatographic fingerprint could provide reference for quality control of acacia honey. 展开更多
关键词 HONEY Volatile components Solid-phase microextraction technology Gas chromatography Fingerprint.
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Ionic liquid based dispersive liquid-liquid microextraction of aromatic amines in water samples 被引量:13
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作者 Yun Chang Fan Zheng Liang Hu +2 位作者 Mei Lan Chen Chao Shen Tu Yan Zhu 《Chinese Chemical Letters》 SCIE CAS CSCD 2008年第8期985-987,共3页
In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4... In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4-aminobiphenyl in aqueous matrices. After extraction the ionic liquid (IL) phase was injected directly into the high performance liquid chromatography (HPLC) system for determination. Some parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. The limits of detection (LOD, S/N = 3) for the four analytes were in the range of 0.45-2.6 μg L^-1. The relative standard deviations (R.S.D., n = 6) were in the range of 6.2-9.8%. This method was applied for the analysis of the real water samples. The recoveries ranged from 93.4 to 106.4%. The main advantages of the method are high speed, high recovery, good repeatability and volatile organic solvent-free. 展开更多
关键词 Ionic liquid (IL) Dispersive liquid-liquid microextraction (DLLME) High performance liquid chromatography (HPLC) Aromatic amines
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Changes of Aroma Components in Hongdeng Sweet Cherry During Fruit Development 被引量:11
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作者 ZHANG Xu JIANG Yuan-mao +3 位作者 PENG Fu-tian HE Nai-bo LI Yan-ju ZHAO Deng-chao 《Agricultural Sciences in China》 CAS CSCD 2007年第11期1376-1382,共7页
To study the changes of aroma components in sweet cherry during fruit development, the aroma components in sweet cherry fruit from the green stage, the color stage, the commercial stage, and the ripe stage were collec... To study the changes of aroma components in sweet cherry during fruit development, the aroma components in sweet cherry fruit from the green stage, the color stage, the commercial stage, and the ripe stage were collected using head-space solid phase microextraction (HS-SPME), and were analyzed using a gas chromatograph-mass spectrophotometer (GC- MS). A total of 37 compounds were identified from the sample extracts. Aldehydes, alcohols, and esters were the major constituents. The aroma components behaved differently during the fruit developmental period. C6 aldehydes and aromatic aldehydes were the main aldehydes in the sweet cherry fruit. The contents of C6 aldehydes increased quickly to 84.16% in the color stage, then decreased as ripening proceeded, and then, the contents decreased to 59.20 and 55.58% at the commercial stage and the ripe stage, respectively. The aromatic aldehydes (benzaldehyde) increased as ripening proceeded, and the maximum was found at the ripe stage. Alcohols of sweet cherry fruit included C6 alcohols and aromatic alcohols. The content of (E)-2-hexen-l-ol increased as ripening proceeded. The maximum was found at the commercial stage; alcohol was only found at the ripe stage. Ester components included ethyl acetate, butanoic acid ethyl ester, hexanoic acid ethyl ester, which increased as the fruit ripened. Hexanal, (E)-2-hexenal, benzaldehyde, (E)-2-hexen-l-ol, ethyl acetate, and hexanoic acid ethyl ester were the characteristic aroma components of sweet cherry fruit. These aroma components started to form drastically at the color stage, and the main aroma was formed at the commercial stage, which then turned bad at the ripe stage because of the presence of alcohol. So the optimal harvest time of sweet cherry was at the commercial stage. 展开更多
关键词 sweet cherry fruit development aroma components solid phase microextraction GC-MS
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固相微萃取GC-MS快速分析火场残留物中汽油成分 被引量:11
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作者 高展 袁春 +1 位作者 刘峰 郑执 《分析测试学报》 CAS CSCD 北大核心 2004年第z1期295-297,共3页
  火场残留物如碳灰、烧残物等通常经过样品预处理后进行分析鉴定.传统的样品预处理方法往往操作繁琐、费时、重复性差,而且需用大量有机溶剂,不利于分析人员的身体健康,对环境也会造成一定污染.……
关键词 Fire debris GASOLINE Solid phase microextraction GC - MS
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Novel method for the determination of five carbamate pesticides in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography 被引量:10
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作者 Zhi Mei Liu Xiao Huan Zang Wei Hua Liu Chun Wang Zhi Wang 《Chinese Chemical Letters》 SCIE CAS CSCD 2009年第2期213-216,共4页
A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) ... A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography-diode array detector (HPLC-DAD). Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients (r^2) varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection (LODs) (S/N = 3) were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples. 展开更多
关键词 Carbamate pesticides High performance liquid chromatography Diode array detection Dispersive liquid-liquid microextraction Water samples
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关于鸡蛋黄、鸭蛋黄、咸鸡蛋黄、咸鸭蛋黄四种蛋黄风味物质的研究 被引量:12
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作者 周芹 李文钊 《中国调味品》 CAS 北大核心 2012年第6期35-39,共5页
咸蛋因其鲜嫩可口,营养丰富是一直深受国内外消费者喜欢的传统美食。尤其是咸蛋黄不仅可以直接食用,还被用于添加至月饼等糕点中,提高产品的口感与营养。鸡蛋、鸭蛋经腌制后产生了更多宜人的口感和风味。文章运用顶空微萃取技术与气质... 咸蛋因其鲜嫩可口,营养丰富是一直深受国内外消费者喜欢的传统美食。尤其是咸蛋黄不仅可以直接食用,还被用于添加至月饼等糕点中,提高产品的口感与营养。鸡蛋、鸭蛋经腌制后产生了更多宜人的口感和风味。文章运用顶空微萃取技术与气质联用相结合的方法对鸡蛋黄、鸭蛋黄、咸鸡蛋黄和咸鸭蛋黄四种蛋黄进行了挥发性风味物质的研究。 展开更多
关键词 鸡蛋黄 鸭蛋黄 挥发性化合物 顶空固相微萃取 气质联用
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酱油挥发性成分固相微萃取条件的优化 被引量:9
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作者 刘非 杜丽平 肖冬光 《食品与发酵工业》 CAS CSCD 北大核心 2017年第7期70-75,共6页
顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)是提取挥发性成分比较常用的方法。为了确定提取酱油挥发性成分的SPME萃取头,分别以挥发性成分的累积峰面积标准化值和峰面积相对标准偏差的平均值与标准偏差为指标,考... 顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)是提取挥发性成分比较常用的方法。为了确定提取酱油挥发性成分的SPME萃取头,分别以挥发性成分的累积峰面积标准化值和峰面积相对标准偏差的平均值与标准偏差为指标,考察了不同型号萃取头的萃取灵敏度和重复性,确定采用65μm PDMS/DVB提取酱油挥发性成分;并以各类挥发性成分峰面积和总峰面积为指标,优化了其萃取条件,确定萃取条件为:样品用量8 m L,萃取温度60℃,萃取时间60 min。利用优化方法对酱油挥发性成分进行提取,经气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)分析,共鉴定出86种挥发性成分,其中最主要的为酯类物质,其次为醇类、醛类和酸类。挥发性成分峰面积的平均相对标准偏差为8.14%,方法重复性较好。 展开更多
关键词 顶空固相微萃取(headspace solid—phase microextraction HS-SPME) 酱油 挥发性成分 灵敏度 重复性 优化
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酱香型大曲的挥发性组分时空性特征的分析 被引量:8
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作者 李登勇 黄钧 +3 位作者 丁晓菲 金垚 吴重德 周荣清 《食品与发酵工业》 CAS CSCD 北大核心 2018年第7期243-249,共7页
6种不同酱香型大曲的理化参数及挥发性组分的研究结果表明,酱香型大曲的挥发性组分具有显著的时空性特征(大曲生产地点和储存时间)。酱香型大曲主要挥发性组分包括芳香族、酯类、含氮化合物等。基于挥发性组分对不同类型的酱香型大曲进... 6种不同酱香型大曲的理化参数及挥发性组分的研究结果表明,酱香型大曲的挥发性组分具有显著的时空性特征(大曲生产地点和储存时间)。酱香型大曲主要挥发性组分包括芳香族、酯类、含氮化合物等。基于挥发性组分对不同类型的酱香型大曲进行主成分分析(principal components analysis,PCA)和聚类分析等统计分析,能有效地辨析其时空性特征。酱香型大曲生产地域之间的差异能够显著改变主要挥发性组分的种类,而相同地域不同生产企业和不同生产地点的酱香型大曲中的挥发性组分含量也差异较大。茅台原产曲的曲心和曲表的含氮化合物类挥发性组分的比例分别是52.83%和22.05%,其中较高的吡嗪类含氮组分是茅台原产曲的重要特征,而源于其他生产域的酱香型大曲中挥发性组分则以酯类为主(51.55%~79.49%)。同时酱曲主要挥性发组分种类及含量因陈曲时间而异。 展开更多
关键词 挥发性组分 酱香型大曲 顶空固相微萃取(headspace solid-phase microextraction HS-SPME)
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固相微萃取-气相色谱法测定废水中三乙胺和苯胺 被引量:10
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作者 宋艳涛 王正萍 王琳 《环境监测管理与技术》 北大核心 2005年第1期37-38,共2页
采用固相微萃取-气相色谱法建立了测定废水中三乙胺和苯胺的方法,对萃取条件和气相色谱条件进行了优化.方法的相对标准偏差为0.5 %~0.8 %,加标回收率为96.3 %~107.0 %.总分析时间小于1 h,适用于快速分析废水中胺类化合物.
关键词 固相微萃取 气相色谱 三乙胺 苯胺
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液液微萃取-甲基衍生化/气相色谱法对水中氯代酸除草剂的测定 被引量:9
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作者 周林军 刘济宁 +3 位作者 石利利 单正军 陈国松 吕凤兰 《分析测试学报》 CAS CSCD 北大核心 2009年第7期829-833,共5页
在pH大于12的条件下使水样中的氯代除草剂全部水解为盐,用正己烷和甲基叔丁基醚混合溶剂提取有机杂质,再在酸性条件下经5mL甲基叔丁基醚提取,重氮甲烷甲基衍生化30min后用带微电子捕获检测器的毛细管气相色谱分析,以4,4’-二溴八... 在pH大于12的条件下使水样中的氯代除草剂全部水解为盐,用正己烷和甲基叔丁基醚混合溶剂提取有机杂质,再在酸性条件下经5mL甲基叔丁基醚提取,重氮甲烷甲基衍生化30min后用带微电子捕获检测器的毛细管气相色谱分析,以4,4’-二溴八氟联苯为内标物进行定量。茅草枯、麦草威、2,4-D、五氯苯酚的质量浓度分别在5.0—500、1.0~200、5.0~500、0.5~100ug/L范围内与色谱峰面积呈良好的线性关系(r=0.9945~0.9980),检出限分别为1.0、0.5、1.0、0.1ug/L。用该法测定南京玄武湖水样中的茅草枯,其质量浓度为7.1ug/L,4种被测组分在高、中和低添加水平下的回收率分别为102%~105%、96%-110%、87%-109%。同时建立了一种生产重氮甲烷的新原料——N-亚硝基-N-甲基脲的简易方法。 展开更多
关键词 氯代酸除草剂 气相色谱 甲基衍生化 微萃取
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提高气相色谱法测定药物残留溶剂灵敏度的方法 被引量:10
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作者 谭必琴 刘雁鸣 《中南药学》 CAS 2016年第8期846-850,共5页
药典中收载的测定残留溶剂的方法一般为静态顶空气相色谱法,但对高沸点残留溶剂此方法灵敏度欠佳,此文对提高残留溶剂测定灵敏度的气相色谱相关方法进行了总结,显示不同顶空溶剂及样品处理方法与气相色谱结合有效提高了残留溶剂检测灵... 药典中收载的测定残留溶剂的方法一般为静态顶空气相色谱法,但对高沸点残留溶剂此方法灵敏度欠佳,此文对提高残留溶剂测定灵敏度的气相色谱相关方法进行了总结,显示不同顶空溶剂及样品处理方法与气相色谱结合有效提高了残留溶剂检测灵敏度。这些方法可为残留溶剂的研究与测定提供参考。 展开更多
关键词 残留溶剂 灵敏度 顶空 微萃取 气相色谱法
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HS-SPME-GC-MS技术分析不同加工阶段的甲鱼腥味成分变化 被引量:7
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作者 王毅 徐艳群 +1 位作者 徐坤 罗自生 《食品与发酵工业》 CAS CSCD 北大核心 2016年第12期189-193,共5页
为研究不同加工方式对甲鱼腥味成分的影响,采用HS-SPME-GC-MS技术对甲鱼预煮、卤制、烘烤不同加工阶段的腥味物质进行分析。结果表明,经NIST/Willey质谱数据库检索和文献对照,新鲜甲鱼共检出48种挥发成分,确定36种成分,包括烃类21种、醛... 为研究不同加工方式对甲鱼腥味成分的影响,采用HS-SPME-GC-MS技术对甲鱼预煮、卤制、烘烤不同加工阶段的腥味物质进行分析。结果表明,经NIST/Willey质谱数据库检索和文献对照,新鲜甲鱼共检出48种挥发成分,确定36种成分,包括烃类21种、醛类12种、醇类化合物5种、芳香类5种、羧酸类3种、酮类1种、酯类1种。其中以己醛的百分含量最多,为29.1%,有青草味;庚醛占10.69%,具有强烈的油脂氧化味;壬醛占12.58%,提供鱼腥味;占2.02%的对二甲苯有刺激味;占2.36%的1-辛烯-3-醇具有土腥味。认为己醛、壬醛、庚醛、1-辛烯-3-醇等共同形成了甲鱼的腥味。通过预煮、卤制、烘烤等加工工艺后,腥味成分已减少至只能检测出己醛和壬醛,且含量都不超过1%。表明经预煮、卤制、烘烤等加工可以有效控制甲鱼的腥味。 展开更多
关键词 甲鱼 HS-SPME-GC-MS(headspace SOLID-PHASE microextraction gas chromatography-mass spectrometer) 加工方式 腥味成分
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分散液液微萃取-反相液液微萃取-扫集-胶束电动色谱法测定红酒中的3种氯酚类物质 被引量:7
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作者 孙建芝 贺晖 刘书慧 《色谱》 CAS CSCD 北大核心 2014年第3期256-262,共7页
建立了分散液液微萃取(DLLME)-反相液液微萃取(RP-LLME)-扫集-胶束电动色谱富集模型,并用于红酒中五氯酚(PCP)、2,4,6-三氯酚(TCP)和2,4-二氯酚(DCP)3种氯酚的测定。实验考察了两步微萃取的萃取参数对氯酚萃取率的影响和... 建立了分散液液微萃取(DLLME)-反相液液微萃取(RP-LLME)-扫集-胶束电动色谱富集模型,并用于红酒中五氯酚(PCP)、2,4,6-三氯酚(TCP)和2,4-二氯酚(DCP)3种氯酚的测定。实验考察了两步微萃取的萃取参数对氯酚萃取率的影响和样品分离富集的电泳条件。最佳萃取条件 DLLME 为:3.5 mL 红酒( pH 3.0,120 g / L NaCl),300μL 正己烷(萃取剂);RP-LLME 为:25μL 0.16 mol / L NaOH(萃取剂)。最佳电泳条件:25 mmol / L NaH2 PO4,100 mmol / L 十二烷基硫酸钠( SDS),30%( v / v)乙腈,pH 2.3;分离电压-15 kV;样品基质为80 mmol / L NaH2 PO4;压力进样20 s×20.67 kPa(3 psi)。PCP 和 TCP 的线性范围为0.5~100μg / L( r≥0.9910), DCP 的线性范围为1.5~80μg / L(r =0.9851)。3种分析物的检出限( S / N =3)为0.035~0.114μg / L,加标回收率为75.2%~104.7%,相对标准偏差≤6.17%。该方法富集倍数高、灵敏度高、重现性好、分析速度快,可为不同样品基质中痕量氯酚污染物及某些弱酸性有机污染物测定提供参考。 展开更多
关键词 分散液液微萃取 反相液液微萃取 扫集 胶束电动色谱 氯酚 红酒 dispersive LIQUID-LIQUID microextraction( DLLME ) reversed phase LIQUID-LIQUID microextraction( RP-LLME ) micellar electrokinetic chromatography ( MEKC ) chlorophenols(CPs)
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Determination of urinary 8-hydroxy-2′-deoxyguanosine by capillary electrophoresis with molecularly imprinted monolith in-tube solid phase microextraction 被引量:6
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作者 Zhang, Shao Wen Zou, Cun Jie +4 位作者 Luo, Nan Weng, Qian Feng Cai, Ling Shuang Wu, Cai Ying Xing, Jun 《Chinese Chemical Letters》 SCIE CAS CSCD 2010年第1期85-88,共4页
Urinary 8-hydroxy-2 -deoxyguanosine(8-OHdG) is an excellent marker of oxidative DNA damage.In this study,employing guanosine as dummy template a novel molecularly imprinted(MIP) monolithic capillary column had been sy... Urinary 8-hydroxy-2 -deoxyguanosine(8-OHdG) is an excellent marker of oxidative DNA damage.In this study,employing guanosine as dummy template a novel molecularly imprinted(MIP) monolithic capillary column had been synthesized,and that was used as medium of in-tube solid phase microextraction(SPME).Coupled with capillary electrophoresis-electrochemical detection(CE-ECD),the system of extraction and detection of 8-OHdG in urinary sample had been developed.Because of its greater phase ratio combined with conv... 展开更多
关键词 Molecularly imprinted monolith In-tube solid phase microextraction 8-Hydroxy-2 -deoxyguanosine(8-OHdG) Electrophoresis Urine
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