• Analytical Science and Technology
• /
• v.16 no.6
• /
• pp.458-465
• /
• 2003

The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

• Journal of the Society of Cosmetic Scientists of Korea
• /
• v.42 no.1
• /
• pp.65-73
• /
• 2016

Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

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

• Journal of Food Hygiene and Safety
• /
• v.35 no.3
• /
• pp.225-233
• /
• 2020

By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R²), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.

• Journal of Korean Society of Environmental Engineers
• /
• v.29 no.6
• /
• pp.689-698
• /
• 2007

A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples. The alkylphenols, chlorophenols and bisphenol A in korean aquatic biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at $-60^{\circ}C$ for 2 hours(freezing filtration method). Also, solid-phase extraction(SPE) was used to XAD-4 and subsequent conversion to isobutoxycarbonyl(isoBOC) or tert-butyldimethylsilyl(TBDMS) derivatives for sensitive analysis with gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM) mode. For isoBOC derivatization and TBDMS derivatization the recoveries were $70.1\sim150.6%$ and $93.8\sim108.3%$, the method detection limit(MDLs) of bisphenol A for SIM were $0.062{\mu}g/kg$ and $0.010{\mu}g/kg$, and the SIM respectively. When these methods were applied to korean aquatic biological samples, the concentrations of the 11 phenolic EDCs were $0.675\sim1.970{\mu}g/kg$.

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

• Analytical Science and Technology
• /
• v.26 no.4
• /
• pp.228-234
• /
• 2013

Methamphetamine is an amine-containing illegal drug and is distributed unlawfully in South Korea. Finding a rapid, convenient and semi-quantitative determination method for methamphetamine is a very important issue in the area of forensic drug testing. As an effort to develop new screening method, the reactions between three organic compounds which are structurally similar to methamphetamine and N-(9-fluorenylmethoxycarbonyloxy) succinimide (FMOC-NHS) were performed on silica gel ($SiO_2$) TLC plates. Three reference compounds were synthesized and used for the identification, comparison and study of the limit of detection (LOD) of the products obtained from a direct reaction on a TLC plate. As a result, FMOC-NHS as a derivatization reagent generated compounds containing highly UV-active functional groups on the TLC plate after reacting with primary- and secondary amines. In the experiment 2D the LOD of amines was in the range of 0.045 and 0.01 mg/mL ($2{\mu}L/spot$), and in 1D the LOD was in the range of 0.002 and 0.007 mg/mL ($2{\mu}L/spot$). The LODs of the compounds tested were dependent on the concentration of the derivatizing reagent.

• Analytical Science and Technology
• /
• v.6 no.1
• /
• pp.9-19
• /
• 1993

Fatty acid salts derived from soap can be transferred into a typical derivative with p-bromophenacyl bromide using crown ether, a catalizer by the solid-liquid phase transfer reaction in nonpolar, aprotic solvents and separated by the reverse phase high performance liquid Chromatography (RP-HPLC) and determined using UV detector. The minimal limit of detection was defined at approximately 10~50ng in accordance with the chain length. The derivatization reaction in the presence of EDTA can be applied mot only to the calcium salts but also to the other various metal salts. The recoveries of fatty acid derivatizations in the absence and presence of the midium containing the yeast extract were obtained $95.4{\pm}1.2$, and $85.2{\pm}2.4%$ respectively. The analytical method would be applicable to determine the biodegradation of fatty acid salts in nature as well as in artificial condition such as shaker flask-medium method.

• Analytical Science and Technology
• /
• v.18 no.6
• /
• pp.453-459
• /
• 2005

Phenol compounds in water were simultaneously analyzed by extractive derivatization. Aqueous solution was controlled to pH 13 with sodium hydroxide, and then $500{\mu}L$ of benzoyl chloride was added to the solution. The solution was shaken for 15 minutes and extracted with diethyl ether and then analyzed using GC/MS-SIM. The calibration curves of phenolic compounds in the range of 0.05 to $5.0{\mu}g/mL$ showed a good linearity having the correlation coefficient of $r^2=0.9915$ and standard deviation of ${\leq}8.5%$, respectively. The recoveries by this method ware 58.4-114.0%.

• Analytical Science and Technology
• /
• v.19 no.1
• /
• pp.107-114
• /
• 2006

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.