• Title/Summary/Keyword: Recoveries

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Determination of Chromium(VI) and Copper(II) in Organic Solvent - Solution by Liquid Core Optical Fiber Spectrophotometry

  • Wang, JuFang;Fen, Minzhao;Wei, Wang;He, Qushe;Wu, Guanyan
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.457-460
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    • 1995
  • A new hollow fiber filled with the lower refractive index liquid as core constructs a liquid core optical fiber(LCOF). The LCOF have been used as colorimetric cell to determine elements Cr and Cu in the presence of 70%- 50% ethanol or 50% dioxane aqueous solution, based on colored complex of Chromium(VI) with Diphenycarbazid(DPC) and copper with Chromaurd S(CAS) respectively. The sensitivity (1/ng/ml) of calibration curve of Cr and Cu are 0.052, 0.017 over the range 0 - 25, 0 - 24(ng/ml) respectively. The Cr in the animal gum and Nation Standard of China are determined with recoveries of 94 - 102%.

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Simultaneous determination of bisphenol A, chlorophenols and alkylphenols by solid-phase extraction and HPLC

  • Lee, Taejoon;Park, Keun-Young;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.30 no.1
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    • pp.20-25
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    • 2017
  • An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

Studies on the Analytical Methods and Quantity of Residual 2,4-D in Imported Fruits (수입 과일중 2,4-D의 잔류분석법 및 잔류량 연구)

  • 홍무기
    • Journal of Food Hygiene and Safety
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    • v.9 no.2
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    • pp.89-94
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    • 1994
  • A simple, safe, and sensitive gas chromatographic method using packed column and electron capture detector to analyze 2, 4-D herbicide in imported lemon, grapefruit, and orange was described and its usefulness evaluated. In this scheme of analysis the acid herbicide was converted into its alkyl esters by an one-step reaction prior to analysis. The herbicide in the fruits was extracted with ethyl acetate and partitioned against dichloromethane for purification, and the extracts finished partitioning were derivatized with alcohol, using sulfuric acid as a catalyst to form the corresponding alkyl derivatives. The analytical scheme studiedwas found to be applicable for the herbicide in the fruits without a column clean-up procedure. The mean recoveries of the herbicide for lemon samples fortified at 0.1 mg/kg and 1.0 mg/kg were 93% and 95%, respectively. The detection limit was 0.5 $\mu\textrm{g}$/kg for 2.4-D methyl ester.

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A Study on the Analytical Method of Trace Metal Ions in Sea Water by Inductively Coupled Plasma - Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 해수중 미량금속의 분석에 관한 연구)

  • Lee, Won;Park, Kyung-Su;Kim, Eun Kyung;Hur, Young-Hoe
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.499-504
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in sea water has been investigated by Inductively Coupled Plasma-Mass Spectrometry. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Recoveries of 99.8% for Cu, 99.6% for Sn, and 97.9% for Bi were obtained for the standard spiked sample. The developed method was applied to analysis of trace metals in sea water.

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Development of a Virus Elution and Concentration Procedure for Detecting Norovirus in Cabbage and Lettuce

  • Moon, Aerie;Hwang, In-Gyun;Choi, Weon-Sang
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.407-412
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    • 2009
  • In this study, a rapid and efficient concentrating procedure that can be used for detecting viruses in vegetables was developed. The Sabin strain of poliovirus type 1 was used to evaluate the efficiency of virus recovery. The procedure included: (a) elution with 0.25 M threonine-0.3 M NaCl pH 9.5; (b) polyethylene glycol (PEG) 8000 precipitation; (c) chloroform extraction; (d) 2$^{nd}$ PEG precipitation; (f) RNA extraction; (g) reverse transcription-polymerase chain reaction (RT-PCR) combined with semi-nested PCR. The overall recoveries by elution/concentration were 29.0% from cabbage and 13.7% from lettuce. The whole procedure usually takes 18 hr. The overall detection sensitivity was 100 RT-PCR units of genogroup II norovirus (GII NoV)/25 g cabbage and 100 RT-PCR units of GII NoV/10 g lettuce. The virus detecting method developed in this study should facilitate the detection of low levels of NoV in cabbage and lettuce.

Comparison of Free Amino Acids in Soybean Paste (Doenjang) by Different Extraction Solvents and Analytical Methods (추출 용매와 분석 기법에 따른 된장의 유리아미노산 비교)

  • Kang, Ok-Ju
    • Korean journal of food and cookery science
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    • v.23 no.1 s.97
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    • pp.150-155
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    • 2007
  • This work was conducted to obtain a rapid, accurate, and precise procedure for free amino acids analysis in Doenjang with HPLC-OPA (high performance liquid chromatography using-phthalaldehyde) and AAA (automatic amino acid analyzer) methods. Different sample extraction procedures among water, 0.1 M perchloric acid, and 0.1% meta-phosphoric acid were also compared. The optimal extraction solvent was 0.1% meta-phosphoric acid for both the HPLC-OPA and AAA methods. Good recoveries for glycine and methionine were observed using the 0.1% meta-phosphoric acid extraction with HPLC-OPA method. Method precisions (% relative standard deviation) for the free amino acids ranged for 1.62% to 8.27%, in which the HPLC-OPA method with water extraction showed the lowest value at 1.62%. Inhibition rates of the free amino acids in Doenjang were greatest with an addition of NaCI at a 1% concentration.

Determination of Glyphosate in Whole Blood by HPLC-fluorescence Detection (HPLC 형광검출법에 의한 Glyphosate의 혈중농도 측정)

  • 이상기;김기욱;양자열;인상환;이수연
    • YAKHAK HOEJI
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    • v.45 no.4
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    • pp.347-351
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    • 2001
  • A rapid and sensitive method for the determination of glyphosate, a phosphated amino acid herbicide, in whole blood is presented. After removal of protein, the whale blood was purified by using the anion exchange resin (Dowex 1), and derivatized with 9-fluorenylmethyl chloroformate (FMCL). Derivatized glyphosate from blood sample was injected onto a Whatman partisil 10SAX column and separated with 0.1M phosphate buffer (pH 2.5) and acetonitrile (ratio=3:1). The high performance liquid chromatography-fluorescence detection gave the detection limit of 86pg and linearity of 0.9999 in the range of 0.25 $\mu$g/ml and 25 $\mu$g/ml. The recoveries of glyphosate added to the blood samples were ranged from 75.3% to 100.4% compared to the samples prepared in water. The derivatized glyphosate was stable at various acidity and temperature. This method has been successfully applied to the blood samples of lethal intoxication with the herbicide glyphosate.

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The Determination of Gold in Assay Process by Thermal Neutron Activation Analysis (試金工程中의 金의 熱中性子에 依한 放射化分析)

  • J.I. Kim;Chong Kuk Kim;W.P. Chang
    • Journal of the Korean Chemical Society
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    • v.7 no.2
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    • pp.165-169
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    • 1963
  • 12 samples from an assay process chain were submitted to qualitative and quantitative neutron activation analysis for the determination of gold. Gold was detected and quantitatively determined in three samples after a chemical separation consisting of solvent extraction and precipitation steps. Recoveries ranged between 81.0 and 93.6% and results of duplicated determinations were reproducible. Quantitative data were obtained from gamma-spectrometric photopeak-area counting. Interference from fast neutron reactions was negligible.

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Multiresidue Analysis of Eight Acaricides in Fruits

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Journal of Applied Biological Chemistry
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    • v.42 no.4
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    • pp.191-196
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    • 1999
  • A multiresidue analytical method was developed for eight acaricides including benzoximate, clofentezine, fenazaquin, fenothiocarb, fenpyroximate, hexythiazox, pyridaben, and tebufenpyrad in four major fruits using high-performance liquid chromatography (HPLC). All the confounds were extracted with acetone from apple, pear, grape, and citrus samples. The extract was diluted with saline water, and n-heaxane partition was followed to recover the acaricides. Florisil column chromatography was employed to further purify the sample extract. HPLC with ultraviolet absorption detection, using an octadecylsilyl column under the isocratic mobile phase of acetonitrile/water mixture, was successfully applied to separate and quantitate all the compounds in the purified extract. Recoveries of the eight acaricides from for fortified samples ranged 86.4~97.0%. Relative standard deviations of the analytical method were all less than 10%. Detection limits of the method were in the range of 0.02~0.05 mg/kg. The proposed method was reproducible and sensitive enough to evaluate the terminal residue of the eight acaricides in the fruit harvest.

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Simultaneous HPLC Determination of Preservatives in Cosmetics (화장품중 살균ㆍ보존제의 동시분리 및 정량)

  • 양성준;김영옥;손경훈;이정표;정래석;양원준;백옥진;이현경;최상숙
    • YAKHAK HOEJI
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    • v.46 no.4
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    • pp.231-236
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    • 2002
  • A high-performance liquid chromatographic method for the simultaneous quantitative analysis of methylparaben (MP), ethylparaben (EP), propylparaben (PP), butylparaben (BP) and imidazolidinyl urea(IU) or diazolidinyl urea(DU) in cosmetics was studied by using a cyano-propyl column and 0.05M hexanesulfonic acid at 228 nm. Calibration curves were found to be linear in the 60-1000 $\mu\textrm{g}$/mL range (parabens), 100-1,250 $\mu\textrm{g}$/mL range (IU) and the 120-2000 $\mu\textrm{g}$/mL range (DU). Linear regression analysis of the data demonstrates the efficacy of the method in terms of precision and accuracy. An extraction method is developed and validated in order to apply this chromatographic method to a commercial cosmetic cream. The precision of this method, calculated as the relative standard deviation (RSD) of the recoveries (0.46-2.71%) was excellent for all compounds.