• 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

• Journal of Korean Society for Atmospheric Environment
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• v.22 no.3
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• pp.297-307
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• 2006

During January $2002{\sim}April\;2004$, hydrogen peroxide ($H_{2}O_{2}$) measurements were performed at the campus of Korea University, which is located in the northeastern part of Seoul. Gas phase hydroperoxide was collected in aqueous solution and separated by HPLC. Concentrations were determined by fluorescence using postcolumn enzyme derivatization. This measurement system was improved to be run automatically from sample collection at every 10 minutes through chemical analysis for data collection. Detection limits of $H_{2}O_{2}$ is $10{\sim}17\;pptv$, and the overall uncertainty of the measurements is better than 8%. Two-year measurements of $H_{2}O_{2}$ show typical seasonal variations. Concentrations of $H_{2}O_{2}$ were higher during $June{\sim}October$ and lower during $January{\sim}February$. Maximum concentration of 1-hour averaged $H_{2}O_{2}$ was 6.5 ppbv, which was observed in August and September. In general $H_{2}O_{2}$ concentrations were well correlated with $O_{3}$ concentrations and largely affected by meteorological factors such as temperature and wind direction.

• Mass Spectrometry Letters
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• v.10 no.1
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• pp.1-10
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• 2019

Amphetamine-type stimulants (ATS) are a group of ${\beta}$-phenethylamine derivatives that produce central nervous system stimulants effects. The representative ATS are methamphetamine and 3, 4-methylenedioxymethamphetamine (MDMA), and abuse of ATS has become a global problem. Methamphetamine is abused in North America and Asia, while amphetamine and 3, 4-methyle nedioxym ethamphetamine (Ecstasy) are abused in Europe and Australia. Methamphetamine is also the most abused drug in Korea. In addition to the conventional ATS, new psychoactive substances (NPS) including phenethylamines and synthetic cathinones, which have similar effects and chemical structure to ATS, continue to spread to the global market since 2009, and more than 739 NPS have been identified. For the analysis of ATS, two tests that have different theoretical principles have to be conducted, and screening tests by immunoassay and confirmatory tests using GC/MS or LC/MS are the global standard methods. As most ATS have a chiral center, enantiomer separation is an important point in forensic analysis, and it can be conducted using chiral derivatization reagents or chiral columns. In order to respond to the growing drug crime, it is necessary to develop a fast and efficient analytical method.

• Journal of the Korean Chemical Society
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• v.39 no.2
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• pp.94-102
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• 1995

S-Hydroxypropyl(PH) ${\beta}$-cyclodextrin(hydrophilic), dialkyl(DA)-cyclodextrin(hydrophobic), trifluoroacetyl(TA) ${\gamma}$-cyclodextrin(intermediate) stationary phases were used for gas chromatographic separation of racemic alcohols and their derivatives. All the alcohols used for this experiment were derivatived by using trifluoro acetic anhydride, acetic anhydride, or trichloro acetic anhydride. It is apparent that the enantioselectivity of the enantiomeric pairs was very dependent on the type of acylation reagent. The best experimental condition of optical resolution of the alcohols and their derivatives was different on the polarity of the solute molecules. The chiral separation was also studied depending on temperature, polarity of the column, and hydrogen bonding ability and steric effect between the alchols and CD stationary phase. The chiral recognition mechanism is dependent not upon the kinds of the chiral stationay phases but upon the derivatization of the racemic alchols.

• Bulletin of the Korean Chemical Society
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• v.32 no.4
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• pp.1170-1178
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• 2011

In the present study, the approach of high accuracy mass measurements for phospholipid identifications was evaluated using a 7 T ESI-FTMS/linear ion trap MS/MS. Experiments were carried out for porcine brain, bovine liver, and soybean total lipid extracts in both positive and negative ion modes. In total, 59, 55, and 18 phospholipid species were characterized in the positive ion mode for porcine brain, bovine liver, and soybean lipid extracts, respectively. Assigned lipid classes were PC, PE, PEt, PS, and SM. In the negative ion mode, PG, PS, PA, PE, and PI classes were observed. In the negative ion mode, for porcine brain, bovine liver, and soybean lipid extracts, 28, 34, and 29 species were characterized, respectively. Comparison of our results with those obtained by other groups using derivatization-LC-APCI MS and nano-RP-LC-MS/MS showed that our approach can characterize PC species as effectively as those methods could. In conclusion, we demonstrated that high accuracy mass measurements of total lipid extracts using a high resolution FTMS, particularly, 7T FTMS, plus ion-trap MS/MS are very useful in profiling lipid compositions in biological samples.

• Journal of the Korean Chemical Society
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• v.39 no.4
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• pp.257-265
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• 1995

Free amino acids were isolated from milk and their absolute amounts were determined by reversed phase high performance liquid chromatography after derivatization with dansyl chloride. The determination of D- and L-amino acids was based on achiral separation on a C18 column. It was found that milk contained totally 41.00 mg DL-amino acids in 100 mL milk. The level of D-amino acids to L-amino acids was determined by a column-switching system combining an achiral reversed phase separation and chiral chelate additive. The chiral separation was carried out with addition of the chiral Cu(N-benzyl-L-proline)2 chelate to the mobile phase in reversed phase liquid chromatography. It was found that the determination of 16 different amino acids is feasible in the milk sample with a C18 column separation and 12 D-amino acids out of the 16 amino acids can be determined via the column-switching system with chiral separation. 2.05% of D-glutamic acid and 2.93% of D-alanine were found in milk.

• Journal of environmental and Sanitary engineering
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• v.21 no.1 s.59
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• pp.35-43
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• 2006

Formaldehyde is important because of their irritant and toxic properties, mutagenicity and carcinogenicity. In this study, liquid chromatography-mass spectrometry (LC-MS) is used for the analysis of formaldehyde after derivatization with 2,4-dinitrophenylhydrazine (DNPH) cartridge. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearity ($r^2$) was 0.9997 when analyte concentration ranges from 25 to $200{\mu}g/l$. The relative standard deviation (%RSD) was 1.25 % for concentration of $200{\mu}g/l$. The minimum detection limit (MDL) was 0.73 ppbv. It was shown that LC-MS method has a great potential for formaldehyde analysis. The results of formaldehyde from the survey of Ban-Woll and Shi-Hwa Industrial Complex samples, the highest level was 6.20, 3.93 ppb, respectively. The highest emission level of formaldehyde at chemical plants in the Ban-Woll' Shi-Hwa Industrial Complex was 5421.25 ppb.

• Analytical Science and Technology
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• v.13 no.4
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• pp.484-493
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• 2000

The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

• Analytical Science and Technology
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• v.35 no.6
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• pp.229-236
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• 2022

Lipidomic analyses of transient breast milk are far more limited than those of other dairy products. As a preliminary analysis of breast milk lipidomes, analytical methods for polar and nonpolar lipids from transient breast milk were developed, and detailed fatty acid profiles were determined in this study. The newly developed methods include solvent fractionation of phospholipids and acyl glycerol, one-pot derivatization to FAMEs and pyridylcarbinol esters, and instrumental analysis, including GC-FID and GC-MS. The results indicate that breast milk contains 16 major common fatty acids with 8-22 carbons. Additionally, 29 minor fatty acids were identified, including odd-numbered fatty acids and branched analogues with 11-23 carbons. Their detailed concentrations in different fractions were measured using the internal standard method. In addition to ordinary fatty acids, breast milk contains several branched fatty acids, including iso/anteiso acids with 15-18 carbons. Structural studies have been performed on selected minor fatty acids via chemical synthesis.

• Analytical Science and Technology
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• v.18 no.4
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• pp.271-277
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• 2005

Urea in blood has been measured as an effective marker for diagnosis of renal function. Urea which is e end-product of nitrogen containing metabolites such as proteins is filtered through glomeruli of kidneys and then excreted as urine. If the renal function is deteriorated, the urea concentration in blood will be increased, from which the healthiness of renal function is judged. In order to improve the confidence of diagnosis results, the results must keep traceability chain to certified reference materials, which was certified by primary reference method. In this study, we proposed isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) as a candidate primary method, in which $15^N_2$-urea is used as an internal reference material. The developed method is highly accurate in principle and is convenient as it does not require cumbersome derivatization. 0.1 mmol/L ammonium chloride was selected as a mobile phase for HPLC because it provided low interference in MS analysis of relatively low molecular weighted urea. HPLC and MS were connected with an electrospray ionization (ESI) interface of positive mode, which provided high sensitivity and reproducibility. The developed method was validated with internationally recognized reference materials, and we have obtained satisfactory results in an international ring trial. The expanded uncertainty calculated according to ISO guide was 1.8% at 95% confidence interval. The developed method is being used as a primary reference measurement method such as for certification of serum certified reference materials (CRMs).