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71.
SDE-GC-ECD分析水体中有机氯农药 总被引:4,自引:0,他引:4
运用单滴溶剂萃取-气相色谱-微池电子捕获检测器(SDE—GC—μECD)联用技术对水体中有机氯农药进行了分析,优化了影响单滴溶剂萃取的多种因素。该方法除了对P,P′-DDD的线性范围在0.4~4ng/mL之间外,其余的七种目标物(α-666,β-666,γ-666,δ-666,P,P′-DDE,0,P′-DDT,P,P′-DDT)线性范围均在0.04~4.0ng/mL之间,相关系数为0.9976~0.9999,回收率范围为83.3%~96.1%,相对标准偏差为2.1%~7.8%。与传统的液液萃取相比,单滴溶剂萃取不仅准确度、精密度相当,而且还具有省时、省溶剂的优点。 相似文献
72.
M. Piñeiro-Iglesias M. Miñones-Vázquez E. Vázquez-Blanco S. Muniategui-Lorenzo P. López-Mahía D. Prada-Rodríguez 《Chromatographia》2002,56(7-8):483-488
Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of
aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation
detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The
best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen
(near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges
(Supelclean
tm
LC-Silica SPE tubes and Sep-Pak? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of
both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector
was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these
cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank
chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially
important when aliphatic hydrocarbons concentrations are lower than 1 μg mL−1. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples. 相似文献
73.
74.
Summary A method for determining histamine in wine by precolumn derivatization with PITC (phenylisothiocyanate) with reversed-phase HPLC and UV detection is reported. Histamine can be determined together with the 24 amino acids within 40 min, or separately in a shorter time (less than 4 min) if a prior solid phase extraction clean-up is used. 相似文献
75.
Anna Rizzolo Patrizia Lombardi Maristella Vanoli Stefano Polesello 《Journal of separation science》1995,18(5):309-314
Capillary GC/sensory analysis was used to judge if dynamic headspace on sliced pulp and on intact fruit, and solvent extraction could collect the “character impact” and the “contributory” aroma compounds in peaches. Capillary GC/sensory data showed that the headspace techniques selectively recovered the “contributory” volatile compounds, which are strictly related to the characteristic odor of the various peach cultivars, whereas solvent extraction better quantified the “character impact” compounds (lactones). 相似文献
76.
77.
Ning Li Chunhui Deng Ning Yao Xizhong Shen Xiangmin Zhang 《Analytica chimica acta》2005,540(2):317-323
In the study, we developed a simple, rapid, sensitive, and inexpensive method for determination of the disease biomarkers of acetone, hexanal and heptanal in human blood. For the first time, derivatization of carbonyls with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine (PFBHA) was combined with headspace single-drop microextractin (HS-SDME) and gas chromatography-mass spectrometry (GC–MS) and applied to the analysis of acetone, hexanal, and heptanal in human blood. At first, acetone, hexanal and heptanal in blood were derivatized with PFBHA and formed oximes in several seconds. Sequentially, the oximes were headspace extracted and concentrated by a microdrop solvent. Finally, the extracted oximes were analyzed by GC–MS. HS-SDME conditions and method validations were studied. Due to needing of only 2 μl organic solvent, short extraction time of 8 min, and simple operation, derivatization-HS-SDME was shown to be a rapid, simple, and inexpensive technique for analysis of acetone, hexanal, and heptanal in human blood. Moreover, it had low detection limit values from 0.24 to 0.62 nM, and good reproducibility (R.S.D. less than 12%). 相似文献
78.
79.
在现有方法基础上对沉积物中磺胺类、喹诺酮类、大环内脂类和四环素类抗生素的提取、富集、净化以及仪器分析方法进行了优化。以EDTA-Mcllvaine缓冲溶液与乙腈(V:V,1:1)混合液作为提取液,利用超声波细胞破碎仪进行超声提取,串联强阴离子交换柱(SAX)和HLB固相萃取柱进行固相萃取(SPE),通过超高效液相/串联质谱(UPLC-MS/MS)测定沉积物中抗生素的含量。抗生素基质加标回收率在56.4%~110%,相对标准偏差为1.1%~24.3%,方法检出限0.0055~0.716 ng/g。本方法有效地提高了沉积物中抗生素的提取效率,并应用于实际样品的测定中。 相似文献
80.
丙醇-氯化钠双水相体系萃取分离铂、钯、铑、金中的铱及其吸收光谱分析研究 总被引:12,自引:0,他引:12
提出了一种丙醇-氯化钠双水相体系萃取铱的分离-吸收光谱分析方法,在HCl介质中基于铱生成三氯亚锡酸络阴离子动力学速率与铂、钯、铑、金差异使铱与铂、钯、铑、金分离,其后在KI介质中萃取铱使其与贱金属基体分离,研究了在丙醇萃取相中铱的吸收光谱分析,并应用于实际样品中铱的测定。 相似文献