共查询到18条相似文献,搜索用时 46 毫秒
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气相色谱-质谱联用法测定烟用香精成分——烟草用香精前处理方法比较 总被引:1,自引:0,他引:1
采用同时蒸馏萃取(SDE)、超声辅助液液萃取(ULLE)和固相微萃取(SPME)3种前处理方法提取HMT-3烟用香精成分,用气相色谱-质谱联用法(GC-MS)进行分析.对3种萃取方法鉴定出的组分作出比较,考察了方法的各自特点.选取了15种烟用香精为代表,分别采用3种萃取方法对不同类型的烟用香精进行提取.结果表明:ULLE操作简便、快速、节能、萃取效率高;SDE法和ULLE法的重现性明显好于SPME法,适合于香精的定量分析,而SPME有较高的灵敏度,更适合香精的定性分析.根据定性和定量的需要、方法的适用性和香精的物理状态,应选取不同的提取方法,从而能够快速、准确地获得样品信息. 相似文献
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固相微萃取-气相色谱/质谱法建立烟用香精指纹图谱 总被引:1,自引:0,他引:1
采用固相微萃取法(SPME)对6批次的烟用HMT-4香精成分进行提取,GC/MS对其进行分析,建立了该香精的GC/MS指纹图谱的研究方法。通过参兑实验考察了色谱指纹图谱用于香精质量控制的可行性。结果表明:SPME法具有操作简便、快速、节能、萃取效率高等特点,适合于烟用香精成分的提取。6批次的HMT-4香精的指纹图谱稳定性好,相似度高,具有很强的特征性和唯一性。通过参兑实验发现色谱指纹图谱能全面、综合、准确地反映烟用香精的质量情况,可以成为烟用香精质量控制的有效手段。 相似文献
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基于液液萃取/气相色谱-质谱法结合自动解卷积-Kováts保留指数法,建立了电子烟液中挥发性成分的检测方法。对提取溶剂种类进行了优化,并依据烟液中香气成分的香气特征,分析果味和烟草味烟液的香韵构成和差异,确定不同果味烟液的特征香气成分。结果表明:(1)以乙醚为提取溶剂能减弱丙三醇对其他组分识别的干扰。(2)自动解卷积法能准确识别共流出组分和低含量组分;Kováts保留指数法提升了化合物识别的准确度。(3)在10种烟草味烟液中检出15种成分,以豆香、焦香香韵化合物为主;在21种果味烟液中检出80种成分,以果香、花香香韵化合物为主,确定了16类果味烟液的特征香气成分。通过随机验证实验,该方法可有效分辨不同果味类型的果味烟液和烟草味烟液。该方法样品用量少、前处理过程简单、样品分析用时短,能满足烟液中香气成分的检测需要,可为果味电子烟液的检验识别和监管提供参考。 相似文献
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采用高温顶空液相萃取再转移的方法,对中药白术中挥发性成分进行萃取分离富集,采用顶空液液萃取/气相色谱-质谱(HS-LP-LPE/GC-MS)联用法进行测定,并与传统水蒸汽蒸馏法(SD)提取的挥发性成分进行对比。对各种测定条件和影响因素进行了考察,最佳萃取条件为:1.0 mL PEG 400为高温萃取剂,样品用量1.2 g,萃取温度120℃,萃取时间60 min,再将萃取剂用1.0 mL正己烷进行反萃取后进行GC-MS分析;采用HS-LP-LPE/GC-MS鉴定了33个组分,占总组分含量93.18%;SD鉴定了31个组分,占总组分含量97.12%。两种方法共同检测到的组分有29个,均以苍术酮(Atractylone)含量最高。结果表明,两种方法所提取的组分基本相同,可用于白术挥发性成分的测定。 相似文献
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采用超声辅助液液萃取-气相色谱-质谱法,建立了烟用香精香料的指纹图谱。以二氯甲烷-乙醇(9+1)混合溶液为萃取溶剂,饱和氯化钠溶液为水相,超声萃取10min,对1187号烟用香精香料样品进样检测。共检出了25个组分,对其中的23个组分进行了定性。11个批次的样品色谱图显示了较高的相似性,并运用主成分分析法(PCA)区分了添加其它香精香料的掺兑样品。方法可以用于考察烟用香精香料的质量。 相似文献
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本文提出了一种基于超声辅助离子液体分散液液微萃取紫外分光光度法测定药物及人血清中氯诺昔康含量的方法。疏水性离子液体1-辛基-3-甲基咪唑六氟磷酸盐([C8mim PF6])被用作萃取剂,在超声的帮助下,不使用分散剂离子液体即可萃取氯诺昔康,萃取率在85.0%以上。对实验条件如萃取剂的种类和用量、萃取时间、萃取温度、溶液p H、离心时间等进行了优化。在优化条件下,工作曲线的线性范围为0.2~15.0μg·m L-1,检测限为0.032μg·m L-1,加标回收率分别为94.5%~99.0%(药物)和92.2%~98.7%(人血清)。用本方法对氯诺昔康药片和加标后的人血清样品进行了测定,结果令人满意。 相似文献
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A novel extraction method, namely dynamic ultrasound-assisted extraction, is investigated. This technique is efficient with respect to both time and solvent consumption because it utilizes ultrasonic energy in dynamic mode during extraction. Polyphenols (chlorogenic acid, esculetin, rutin, scopoletin, and quercitrin) are extracted from a tobacco (Nicotina tobaccum L.) sample for 10 min with 6 mL of solvent. Fresh solvent is continuously pumped through the sample, with which the analytes can be rapidly extracted, and the possibility of degradation efficiently avoided. Methanol involving 0.5% w/v ascorbic acid was used as extraction solvent; optimal flow rate and extraction time were investigated. The extract was cleaned up by C18 disposable cartridge. The spiked and nonspiked tobacco samples were used for the evaluation of the proposed method. Recoveries obtained were varied from 96 to 108% and RSDs from 2.0 to 4.6%. This extraction technique was revealed to recover larger amounts of polyphenols from tobacco, compared to the static ultrasound-assisted extraction method. 相似文献
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In the present study, a new method using microwave-assisted solvent extraction (MASE) technique followed directly GC analysis was developed for the extraction of volatile organic acids (VOAs) in tobacco. The MASE conditions (heating time, volume of extracting solvent and extraction temperature) were optimized by means of an orthogonal array design (OAD) procedure. The results suggested that extractant, temperature and heating time were statistically the most significant factors. The extracts were directly analyzed with capillary GC operating in splitless-injection mode on an Agilent HP-FFAP capillary column. Under optimum operating conditions, MASE showed significantly better recoveries than those obtained by the conventional extraction method (ultrasonic and reflux extraction), ranging from 90.6% to 103.2%. In addition, a drastic reduction of the extraction time (20 min versus 4 h) and solvent consumption (20 mL versus 100 mL) was achieved with an outstanding reproducibility (CV ≤5%). 相似文献
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The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated
and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time,
reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction,
ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied
to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing
sterols since it gives a higher extraction efficiency than other methods. 相似文献
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蒸馏-萃取法与溶剂萃取法提取杏果实香气成分的比较 总被引:8,自引:0,他引:8
采用水蒸气蒸馏一萃取法和溶剂萃取法提取杏果香成分,用气相色谱一质谱联用测定其化学成分和质量分数,并对两种提取方法进行了比较。水蒸气蒸馏一萃取法提取的杏果香成分是74种,占总峰面积的73.604%;溶剂萃取法提取的杏果香成分是32种,占总峰面积的44.677%,两者相同的成分有21种。溶剂萃取法提取的主要是烷烃类化合物,水蒸气蒸馏萃取法提取的主要化合物为G醛类、C6醇类、内酯类、萜烯醇类、酮类、烷烃类等。结果表明:水蒸气蒸馏-萃取法能较好地提取杏果实香气成分。 相似文献
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Supercritical fluid extraction of flumetralin in tobacco 总被引:2,自引:0,他引:2
Summary This work evaluates the level of Flumetralin residues in real tobacco samples. Conventional extraction methods were compared with SFE methods in both static and dynamic modes using CO2 and CO2 with modifier. Additionally, in the dynamic SFE mode, different collection approaches, such as collection at room temperature without solvent, collection at room temperature in the presence of solvent (hexane) and collection in an ice bath, without solvent, were studied. SFE showed itself to be a promising extraction technique for pesticide residues in tobacco samples. 相似文献
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Chimuka L van Pinxteren M Billing J Yilmaz E Jönsson JÅ 《Journal of chromatography. A》2011,1218(5):647-653
A selective extraction technique based on the combination of membrane assisted solvent extraction and molecularly imprinted solid phase extraction for triazine herbicides in food samples was developed. Simazine, atrazine, prometon, terbumeton, terbuthylazine and prometryn were extracted from aqueous food samples into a hydrophobic polypropylene membrane bag containing 1000μL of toluene as the acceptor phase along with 100mg of MIP particles. In the acceptor phase, the compounds were re-extracted onto MIP particles. The extraction technique was optimised for the type of organic acceptor solvent, amount of molecularly imprinted polymers particles in the organic acceptor phase, extraction time and addition of salt. Toluene as the acceptor phase was found to give higher triazine binding onto MIP particles compared to hexane and cyclohexane. Extraction time of 120min and 100mg of MIP were found to be optimum parameters. Addition of salt increased the extraction efficiency for more polar triazines. The selectivity of the technique was demonstrated by extracting spiked cow pea and corn extracts where clean chromatograms were obtained compared to only membrane assisted solvent extraction or only molecularly imprinted solid phase extraction. The study revealed that this combination may be a simple way of selectively extracting compounds in complex samples. 相似文献
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比较了烟叶中油分的萃取方法,分别采用超声、索氏、ASE加速溶剂和CO2超临界萃取方法萃取烟叶中的油分,萃取物再经硅胶氧化铝柱分离成3种不同极性的馏分,馏分使用气相色谱分离,质谱鉴定结构.在同时考虑萃取率和萃取物组成成分的基础上最终选择索氏萃取.通过对萃取溶剂和萃取时间进行单因素试验,确定了最佳萃取条件为:萃取溶剂三氯甲烷,萃取时间16 h.方法所得组分全面,有利于后期卷烟配方的调整与设计. 相似文献
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《Journal of separation science》2017,40(22):4366-4376
The volatile organic compound profile in beer is derived from hops, malt, yeast, and interactions between the ingredients, making it very diverse and complex. Due to the range and diversity of the volatile organic compounds present, the choice of the extraction method is extremely important for optimal sensitivity and selectivity. This study compared four extraction methods for hop‐derived compounds in beer late hopped with Nelson Sauvin. Extraction capacity and variation were compared for headspace solid‐phase micro extraction, stir bar sorptive extraction, headspace sorptive extraction, and solvent‐assisted flavor evaporation. Generally, stir bar sorptive extraction was better suited for acids, headspace sorptive extraction for esters and aldehydes, while headspace solid‐phase microextraction was less sensitive overall, extracting 40% fewer compounds. Solvent‐assisted flavor evaporation with dichloromethane was not suitable for the extraction of hop‐derived volatile organic compounds in beer, as the profile was strongly skewed towards alcohols and acids. Overall, headspace sorptive extraction is found to be best suited, closely followed by stir bar sorptive extraction. 相似文献