• Analytical Science and Technology
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• v.28 no.2
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• pp.79-85
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• 2015

A preliminary experiment was performed to develop a fast, convenient, and economical semi-quantitative method of analyzing amphetamine-like amines from images of derivatives. These were generated from the reaction (in situ, co-spot) of three amphetamine-like compounds with three derivatization reagents on a TLC plate. The attempt was made to optimize the reaction conditions for an efficient derivatization reaction, and TLC images taken by a digital camera were analyzed using two types of image analysis program (CP Atlas 2.0 and ImageJ) for repeatability (RSD, %) and linearity (R²). Then, their results were compared. For efficient derivatization, the reaction conditions needed to be modified. The results of image analysis of each of the samples at two different concentrations (0.5 mg/mL and 0.01 mg/mL) showed that the RSD values for reaction repeatability were in the range of 0.69-5.50%. From the calibration curves between the area of the derivative and the concentration of amines, the R² values (R² > 0.9906) for good linear correlation were found to be high, in a concentration range of 0.1-0.005 mg/mL of amines. In addition, the two programs demonstrated little difference in the analysis of repeatability and linearity of the derivatization, so that the current method has the potential to be used for the semi-quantitative analysis of amines.

• Environmental Analysis Health and Toxicology
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• v.15 no.3
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• pp.107-113
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• 2000

Chlorophenoxy acids are one of the most useful classes of chlorinated herbicides. Specially 2, 4-D and 2, 4, 5-T were known to endocrine distruptors. In this study, these pesticides in water samples were extracted by liquid-liquid extration at acidic conditions and then derivatization of acidic group was carried out various esterifications using by CH$_3$I/Acetone -K$_2$CO$_3$, H$_2$SO$_4$/MeOH or TFAA/TFE. That result, Sensitivities of TFE derivatized 2, 4-D and 2, 4, 5-T are prior to the others. The recoveries of 2, 4-D and 2, 4, 5-T were 98% and 82% respectively using diethyl ether as an extracting solvent.

• Analytical Science and Technology
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• v.12 no.6
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• pp.571-576
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• 1999

Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

• Analytical Science and Technology
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• v.15 no.3
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• pp.221-228
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• 2002

AMX is one of extremely high mutagenic compound produced from the reaction of the chlorine and the organic compound during the disinfection of tap water. In this paper, the chemical derivatization of MX with 2% sulfuric acid-methanol, iso-propanol, sec-butanol and n-butanol derivatives for the GC/MS analysis were tested or compared. Limit of detection for the EI and NCI mode were 25 pg and 1.25 pg, respectively. The good linear calibration curve was obtained the range of 25~2500 pg by EI and NCI

• Analytical Science and Technology
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• v.16 no.5
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• pp.349-357
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• 2003

The universality of low molecular weight metabolites (i.e. amino acids, steroid hormones) allows rapid and straightforward investigation of biochemistry of genetically un-characterized species. Thus in vivo metabolic profiling of amino acid in combination with multivariate data analysis (metabolomics) offers great potential in comparative biology. In this paper, amino acid profiles in biological fluid (media) were studied by using HPLC/FLD. HPLC procedure for amino acids require the formation of derivatives due to the low absorption of the free compounds. o-Phthalaldehyde (OPA) used in association with a thiol, such as 3-mercaptopropionic acid (3-MPA), is one of the most popular and sensitive reagents, which yield quickly fluorescent iso-indoles at room temperature. To improve unstability of OPA/3-MPA derivatization, we optimized injector programs for fixed injection times. Linear regressions for the standard curves were linear in the range 0.5 - 100.0 ppb, giving correlation coefficents above 0.99. The detection limit were 1.70 pmol(GLU) - 23.81 pmol(SER). It is practically useful when the amount of sample is very low on single cells.

• Analytical Science and Technology
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• v.26 no.1
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• pp.19-26
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• 2013

Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.

• Journal of Korean Society of Environmental Engineers
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• v.37 no.2
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• pp.81-86
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• 2015

A simple analytical method to quantify formaldehyde in water at lower levels (${\mu}g/L$) was developed using a high performance liquid chromatography (HPLC) and acetylacetone as a derivative reagent. Unlike conventional methods, no extraction and/or concentration were required. The derivative reagent was added into samples and reacted for 30 minutes at $80^{\circ}C$ prior to the analysis of formaldehyde using HPLC. The method detection limit and the limit of quantification for this method were 1.6 and $5.0{\mu}g/L$, respectively. This method also achieved high precision (0.6-3.0%) and accuracy (91.6-106.3%). The recovery rates for various environmental samples ranged from 92.0 to 115.2%.

• Analytical Science and Technology
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• v.17 no.4
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• pp.322-336
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• 2004

The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

• Analytical Science and Technology
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• v.9 no.2
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• pp.198-202
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• 1996

A rapid and simple method for the determination of histamine by reverse-phase high performance liquid chromatography with fluorescence detection was established. 9-Fluorenylmethyl chloroformate(FMOC) was used as fluorescent derivative reagent. The optimum conditions for the derivatization such as pH, reaction time and the concentration of FMOC were investigated. Linearity of calibration curve was obtained between $0.1{\mu}g/ml$ and $0.5{\mu}g/ml$(r=0.992) and the limit of detection was $0.01{\mu}g/ml$.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.360-365
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• 2007

The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 ${\mu}g/kg$ which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 ${\mu}g/kg$ on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 ${\mu}g/kg$ by GC/ECD and GC/MSD, respectively.