A method was developed for the analysis of ester-linked phenolic acids in forage samples using extraction by an ultrasound-assisted treatment and quantification by HPLC with a UV-VIS detector. A reversed-phase C18 col...A method was developed for the analysis of ester-linked phenolic acids in forage samples using extraction by an ultrasound-assisted treatment and quantification by HPLC with a UV-VIS detector. A reversed-phase C18 column was used for developing the method and the optimal condition was established with isocratic elution using acetonitrile/methanol/H3PO4 pH 2.08 (13:12.5:74.5) as the mobile phase. To reduce the time of sample processing, the extraction of ester-linked phenolic acids was studied using ultrasound bath and the results were then compared with those from an extraction usual using alkaline hydrolysis (20°C for 24 h). The method was valued through external and internal calibration. Internal calibration using o-coumaric acid as internal standard and m-coumaric acid as surrogate internal standard showed better results. The detection limits were of 0.09 and 0.04 mg●L-1 for p-coumaric and ferulic acids, respectively. The proposed method showed a good linear dynamic range (3.00 - 30.00 mg●L-1) for the analytes. The usefulness of the methodology was demonstrated by addition-recovery experiments using forage samples and values were in the 83 to 99% range. The extraction of ester-linked phenolic acids by 120 minutes of ultrasound bath was faster and more reproducible than alkaline hydrolysis (20°C for 24 h).展开更多
The external calibration in conjunction with internal standardization（ECIS） coupled with laser-induced breakdown spectroscopic（LIBS） technique was proposed to perform the quantitative analysis of Fe content in iro...The external calibration in conjunction with internal standardization（ECIS） coupled with laser-induced breakdown spectroscopic（LIBS） technique was proposed to perform the quantitative analysis of Fe content in iron ore The plasma temperature and the electron number density were calculated to prove that the plasma was under local thermodynamic equilibrium（LTE） conditions and to ensure that the integral intensities of Fe I lines were reasonable. In addition, the result of the quantitative analysis shows a content of （20.26±0.59）% by mass of Fe in the iron ore. It was determined by four calibration curves, drawn for four emission lines of Fe I（373.48, 373.71,404.58 and 438.35 nm） normalized by Mn I line, base on the ECIS method which can eliminate the influence of matrix effect and improve the accuracy of quantitative analysis, compared with the standard addition method. Both the results of these two analytical methods were compared with that listed in the Standard Substance Certificate. The percentage content of Fe in the same sample of iron ore by the ECIS method was （20.17±0.08）% by mass, which shows a good performance to analyze the Fe content of iron ore in combination with LIBS.展开更多
基金the FAPEMIG(Fun-dacao de Amparo a Pesquisa do Estado de Minas Gerais),CNPq(Conselho Nacional de Desenvolvimento Cien-tifico e Tecnologico),CAPES(Coordenacao de Aper-feicoamento de Pessoal de Nivel Superior)and PRO-PESQ/UFJF(Pro-Reitoria de Pesquisa da Universi-dade Federal de Juiz de Fora)for financial support
文摘A method was developed for the analysis of ester-linked phenolic acids in forage samples using extraction by an ultrasound-assisted treatment and quantification by HPLC with a UV-VIS detector. A reversed-phase C18 column was used for developing the method and the optimal condition was established with isocratic elution using acetonitrile/methanol/H3PO4 pH 2.08 (13:12.5:74.5) as the mobile phase. To reduce the time of sample processing, the extraction of ester-linked phenolic acids was studied using ultrasound bath and the results were then compared with those from an extraction usual using alkaline hydrolysis (20°C for 24 h). The method was valued through external and internal calibration. Internal calibration using o-coumaric acid as internal standard and m-coumaric acid as surrogate internal standard showed better results. The detection limits were of 0.09 and 0.04 mg●L-1 for p-coumaric and ferulic acids, respectively. The proposed method showed a good linear dynamic range (3.00 - 30.00 mg●L-1) for the analytes. The usefulness of the methodology was demonstrated by addition-recovery experiments using forage samples and values were in the 83 to 99% range. The extraction of ester-linked phenolic acids by 120 minutes of ultrasound bath was faster and more reproducible than alkaline hydrolysis (20°C for 24 h).
基金Supported by the China Instrumentation Program（No.2011YQ030113） and the National Natural Science Foundation of China （Nos.21175106, 21375105）.
文摘The external calibration in conjunction with internal standardization（ECIS） coupled with laser-induced breakdown spectroscopic（LIBS） technique was proposed to perform the quantitative analysis of Fe content in iron ore The plasma temperature and the electron number density were calculated to prove that the plasma was under local thermodynamic equilibrium（LTE） conditions and to ensure that the integral intensities of Fe I lines were reasonable. In addition, the result of the quantitative analysis shows a content of （20.26±0.59）% by mass of Fe in the iron ore. It was determined by four calibration curves, drawn for four emission lines of Fe I（373.48, 373.71,404.58 and 438.35 nm） normalized by Mn I line, base on the ECIS method which can eliminate the influence of matrix effect and improve the accuracy of quantitative analysis, compared with the standard addition method. Both the results of these two analytical methods were compared with that listed in the Standard Substance Certificate. The percentage content of Fe in the same sample of iron ore by the ECIS method was （20.17±0.08）% by mass, which shows a good performance to analyze the Fe content of iron ore in combination with LIBS.
