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Determination of phthalate esters in liquor samples by vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction followed by GC–MS
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Geng Leng Wenjin Chen Mingfang Zhang Fang Huang Qiming Cao 《Journal of separation science》2014,37(6):684-690
A novel method using vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction has been developed for the extraction of phthalate esters (PAEs) in Chinese liquor samples prior to analysis by GC–MS. In the proposed method, a high‐density extraction solvent (carbon tetrachloride) was dispersed into samples with the aid of a surfactant (Triton X‐100) and vortex agitation, resulting in a short extraction equilibrium (30 s). After centrifugation, a single microdrop of solvent was easily collected for GC–MS analysis. Key factors that affected the extraction efficiency were optimized. Under the optimum conditions, linearity was found in the range from 0.05 to 50 μg/L. Coefficients of determination varied from 0.9938 to 0.9971. LODs, based on an S/N of 3, ranged from 4.9 to 13 ng/L. Enrichment factors varied from 140 to 184. Reproducibility and recoveries were assessed by testing a series of three liquor samples that were spiked with different concentration levels. Finally, the proposed method was successfully applied to the determination of PAEs in 16 Chinese liquor samples. In this work, high‐density‐solvent vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction was applied for the first time for the extraction of PAEs in Chinese liquor samples and was proved to be simple, rapid, and sensitive. 相似文献
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提出了同位素稀释-气相色谱-质谱法测定白酒中23种邻苯二甲酸酯类化合物含量的方法。样品用正己烷-乙酸乙酯(1+1)混合液提取后,经DB-5MS毛细管色谱柱分离,采用电子轰击离子源选择离子反应监测模式进行质谱测定,同位素内标法进行定量分析。23种邻苯二甲酸酯类化合物的线性范围在0.2~3.0mg·L-1之间,测定下限(10S/N)在0.05~0.1mg·kg-1之间。加标回收率在73.2%~122%之间,相对标准偏差(n=6)在0.49%~11%之间。 相似文献
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火焰原子吸收法测定氰化镀银液中的铜和铁 总被引:2,自引:0,他引:2
提出了用火焰原子吸收光谱法测定氰化镀银液中铜、铁含量的方法,在测定条件下,其他共存元素均无干扰。该方法的相对标准偏差为铜(1.92%-2.63%、铁3.13%-3.73%,样品加标回收率为铜96.8%-101.6%、铁97.5%-101.1%。 相似文献
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Gerhard Triebig Klaus Goßler Margareta Klinger 《Fresenius' Journal of Analytical Chemistry》1979,299(4):271-272
Summary A simple and reliable micromethod is described for the quantitative determination of Chloramphenicol in serum and cerebrospinal fluid (CSF) using high-pressure liquid chromatography. A precipitation of protein while preparing the sample is the important simplification of this method. The detection limit was 0.5 mg of chloramphenicol/l body fluid; the coefficient of variation within series was calculated to be 3.1%; the recovery rate was 55%.
Mikroverfahren zur Bestimmung von Chloramphenicol in Körperflüssigkeiten durch HPLC
Zusammenfassung Es wird eine einfache und zuverlässige Mikromethode zur quantitativen Bestimmung von Chloramphenicol in Serum und Liquor mit Hilfe der Hochdruck-Flüssigkeits-Chromatographie beschrieben. Als entscheidende Vereinfachung liegt diesem Verfahren nur eine Eiweißfällung als Probenvorbereitung zugrunde. Die Nachweisgrenze beträgt 0,5 mg Chloramphenicol/l Körperflüssigkeit, der Variationskoeffizient in der Serie errechnet sich zu 3,1%. Die Wiederauffindungsrate war 55%.相似文献
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叶国源 《理化检验(化学分册)》2014,(11):1401-1404
应用气相色谱-质谱法测定酒中16种邻苯二甲酸酯的含量。样品经乙酸乙酯提取,所得提取液用DB-5MS UI色谱柱分离,在全扫描/选择离子监测共用模式下测定。16种邻苯二甲酸酯的质量浓度均在0.5~10.0mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.01~0.10mg·L-1之间。日间加标回收率在83.7%~114%之间,日间相对标准偏差(n=6)在3.4%~9.8%之间;日内加标回收率在81.9%~113%之间,日内相对标准偏差(n=6)在1.5%~6.7%之间。 相似文献
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酿造酒的激光拉曼光谱 总被引:3,自引:0,他引:3
用激光拉曼光谱的方法对市场销售的几种酿造酒进行了研究,对酿造酒的拉曼光谱的归属进行了设定,并指出了拉曼光谱对鉴别酒的质量所具有的意义 相似文献
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Mansoor Iqbal Zeeshan Khatri Aleem Ahmed Javaid Mughal Kamran Ahmed 《Journal of Saudi Chemical Society》2012,16(1):1-6
Reactive dyeings were carried out by exhaust method on 100% cotton knits. A trichromatic combination was chosen with only change in blue component. Colorimetric data were produced under controlled dyeing conditions by comparing the color difference between the target shade and resulting shades. Giving a change in liquor ratio and nature of salt the colorimetric data were regenerated again produced the shades. The data will be helpful to predict the low-sensitivity reactive dye recipe, which lead to the concept of right-first-time dyeing. The aim of this research is to help a dyer to select the right recipe. A set of the dye recipes was applied by dyeing with reactive dyes on cotton. Sodium chloride shows best results in terms of dye sensitivity as compared to Glauber's salt at low liquor ratio that is 1:10. Blue BRF in combination with yellow and red shows best result as compared to navy blue BF. 相似文献