• Analytical Science and Technology
• /
• v.10 no.5
• /
• pp.343-349
• /
• 1997

Analytical method using the reversed phase ion-pair chromatography (RP-IPC) for the determination of kasugamycin(5-amino-2-methyl-6-(2,3,4,5,6-pentahydroxy cyclohexyloxy)tetrahydropyran-3-yl-amino-${\alpha}$-imino acetic acid), pesticide as fungicide bactercide has been established. The retention behavior of kasugamycin in the RP-IPC was examined with respect to the effect of concentrations of organic modifiers, pH of eluent and types and concentrations of the counter ions as ion-pair reagent. This method developed by the optimum factors, can be used for the application of the quality control in the crude product and its formulation.

• Analytical Science and Technology
• /
• v.33 no.1
• /
• pp.23-32
• /
• 2020

Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

• Analytical Science and Technology
• /
• v.36 no.5
• /
• pp.216-223
• /
• 2023

Aluminium (Al) is one of the major elements in rocks and its concentration can be varied, depending on different rock types as well as sources. The present study aimed to propose an analytical method based on the UV-Vis as a cheap, simple, and common instrument equipped in most laboratories for Al quantification in rocks after the microwave assisted acid digestion. The aluminone and 8-hydroxyquinoline were investigated for the colorimetric assay. The results show that the 8-hydroxyquinoline reagent was more favorable in terms of the minimized affects of the potential interferences present in the digested solutions, i.e., Fe³⁺, Si⁴⁺ and F^-. The calibration curve was constructed from 0.10 mg/L to 3.00 mg/L with the goodness of linearity (R² = 0.9996). The limits of detection and quantification (LOD and LOQ) were estimated, i.e., 0.029 mg/L and 0.087 mg/L, respectively. The 8-hydroxyquinoline was applied to real rock samples, demonstrating favorable precision (RSD = 0.34 %-1.8 %) and no remarkable differences were found compared to the inductively coupled plasma-mass spectrometry (ICP-MS) as a reference measurement approach.

• Journal of the Korean Society of Tobacco Science
• /
• v.2 no.2
• /
• pp.38-43
• /
• 1980

The spectrophotometric determination oi reducing sugar in the tobacco leaves was carried out by employing blue tetrazolium chloride as a color developing reagent. The absorption maximum of formazan dye which is the product of the reaction between blue tetrazolium chloride and fructose was shown to be $530^{nm}$. In the fructose concentration range of 0.02mg/ml-0.14mg/ml the calibration curve was well coincided to the law of Beer-Lambert. In order to take a look at the accuracy and/or recovery rate of fructose determination, the standard fructose was added to the tobacco leaves and the concentration of this standard fructose was estimated. A tittle lower concentration of the standard fructose compared with the pure one in solution was observed. However, an excellent analytical recovery was revealed under the -2% of relative error limit. When we carried out the quantitative determination of this reducing sugar by the method of visual read-out (without using the spectrophotometer), the relative error was obtained to be $\pm$10%.

• Journal of Korean Society of Water and Wastewater
• /
• v.27 no.6
• /
• pp.827-836
• /
• 2013

Due to the stringent drinking water quality, formaldehyde will be included in Korean drinking water standard from year 2014. However, its standard analytical method has not yet been established. This study compares two analytical methods, DNPH-LC and ACFAS with respect to their analysis principles, Method Detection Limit (MDL), Limit Of Quantitation(LOQ), precision, accuracy, reproducibility, convenience, number of samples analyzed per hour and analysis cost. These methods measure absorption intensity at 360 nm by using HPLC after DNPH-derivatization (DNPH-LC) and at 410 nm by using Automated Continuous Flow Absorption Spectrophotometer (ACFAS), respectively. Reproducibility was tested by repeating the analysis 7 times using a standard solution for each method. For DNPH-LC method, MDL was $0.5{\mu}g/L$, LOQ was $1.58{\mu}g/L$ with standard deviation of $0.16{\mu}g/L$. For ACFAS method, they were $0.27{\mu}g/L$, $0.85{\mu}g/L$L with standard deviation of $0.09{\mu}g/L$, respectively. Both methods satisfied the requirement set by the Korean drinking water quality standard. Complexity of sample pretreatment procedure for DNPH-LC method may cause large error and, consequently, the analytical result will depend on the level of skill of analyst. In contrast, ACFAS method which used only one reagent equipped with an automated injection device showed little analytical error. It costs about $5.00 and $1.00 for one sample to analyze by the DNPH-LC method and the ACFAS method, respectively. Compared to the DNPH-LC method, ACFAS method provided more reliable analytical results. In terms of convenience, easiness and analytical cost, ACFAS method was demonstrated to be superior to the DNPH-LC method. The results of this study suggested that the ACFAS method could be adapted as a proper method for determining formaldehyde content in drinking water.

• Journal of Food Hygiene and Safety
• /
• v.38 no.5
• /
• pp.319-331
• /
• 2023

Aminoglycoside antibiotics, also known as aminoglycosides (AGs), are veterinary drugs effective against a wide range of gram-negative and gram-positive bacteria. Owing to their recent use in cultured meats, it has become essential to establish an analytical method for safety management. AGs are highly polar compounds, and ion-pair reagents (IPRs) are used to ensure component separation. Owing to the high possibility of potential mechanical problems resulting from IPR addition to the mobile phase, an analytical method in which IPRs are added directly to the vial was explored. In this study, methods for analyzing 10 AGs via liquid chromatography-tandem mass spectrometry (LC-MS/MS) with the addition of two IPRs were validated for selectivity, detection limit, quantitation limit, recovery, and precision. The detection limit was 0.0001-0.0038 mg/kg, the quantification limit was 0.004-0.011 mg/kg, and the linearity (R²) within the concentration range of 0.01-0.5 mg/kg was over 0.99. Recovery and precision (expressed as relative standard deviation) evaluated in the two matrices (beef and cell culture media) ranged from 70.7% to 120.6% and 0.2% to 24.7%, respectively. The validated AG analytical method was then applied to 15 meats prepared from chicken, beef, and pork, and 6 culture media and additives used in cultured meat. No AGs were detected in any of the 15 meats distributed in Korea; however, streptomycin and dihydrostreptomycin were detected at levels ranging from 695.85 to 1152.71 mg/kg and 6.35 to 11.11 mg/kg, respectively, in the culture media additives. The LC-MS/MS method coupled with direct addition of IPRs to the vial can provide useful basic data for AG analysis and safety evaluation of meats as well as culture media and additives for cultured meats.

• 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.30 no.6
• /
• pp.303-311
• /
• 2017

A new method for obtaining the photoluminescence of footwear impression by using 1,2-indandione (1,2-IND) solution, which is a latent fingerprint-developing reagent, was studied. A binary complex of DL-alanine and 1,2-IND was prepared by spraying a DL-alanine solution and the 1,2-IND solution (an amino acid sensitive reagent) onto dry or wet origin footwear impression deposited on the surface of printed A4 paper. This binary complex reacts with the trace metal component in the footwear impression to form a ternary complex that exhibits photoluminescence. However, when 5-methylthioninhydrin (5-MTN) solution was used instead of 1,2-IND, no consistent photoluminescence was observed even under identical treatment conditions. In addition, when footwear impressions treated with DL-alanine and 1,2-IND solutions were stored under various temperature conditions (30, 40 and $50^{\circ}C$) and various humidity conditions (30 %, 40 %, 50 % and 60 % RH), the contrast between the footwear impression and the background decreased. Optimal footwear impression photoluminescence was obtained when the footwear impressions treated with DL-alanine and 1,2-IND solutions were stored at $30^{\circ}C$ and 30 % RH for 1 h. The sensitivity of the developed method was ccompared with the sensitivities of three known methods - black gelatin lifting, 2,2'-dipyridyl treatment, and 8-hydroxyquinoline treatment. The results showed that the sensitivity of the developed method was worse than that of the black gelatin lifting method but better than that of 2,2'-dipyridyl or 8-hydroxyquinoline treatment method.

• Analytical Science and Technology
• /
• v.30 no.6
• /
• pp.312-318
• /
• 2017

The shelf life of 1,2-indandione/zinc (1,2-IND/Zn) solution and polyvinylpyrrolidone (PVP) solution, which are known as reagents for developing latent fingermarks deposited on the surface of thermal paper, was studied. The standard latent fingermarks used for comparisons were artificial latent fingermarks printed on thermally sensitive and non-sensitive surfaces with the same intensity. Upon treatment of standard latent fingermarks with the pre-mixed 1,2-IND/Zn and PVP solutions, the fingermarks could be successfully developed until 3 days after the preparation of the mixture. However, from the third day after mixing the reagents, blackening was observed on the surface of the thermal paper, indicating deterioration of the reagent performance. The 1,2-IND/Zn and PVP solutions separately stored without mixing in advance were mixed immediately before use, and the development efficiency of the latent fingermarks deposited on the surface of thermal paper was observed. The performance of the PVP solution decreased after 20 days from the preparation of the reagent. It was also found that the shelf life of 1,2-IND/Zn and PVP mixture was determined by the PVP solution. The effect of oxygen and moisture on the degradation of PVP was investigated. It was found that the performance of the PVP solution deteriorated because of the influence of moisture, though it was not affected by oxygen.

• Analytical Science and Technology
• /
• v.19 no.5
• /
• pp.433-440
• /
• 2006

A HPLC/UV method was developed and validated for the rapid and simultaneous determination of urinary metabolites of organic solvents, mandelic acid, hippuric acid, phenylglyoxylic acid, ortho-, meta- and para-methylhippuric acid, using a monolithic column. The mobile phase was composed of tetrabutylammonium bromide as ion-pairing reagent with a flow rate of 2.4 mL/min. The total run time was less than 2.5 min for all six analytes. Good linearities were obtained for all the metabolites with correlation coefficients above 0.9993. Intra-day precision, accuracy and inter-day precision was 0.01~7.32%, 83.9~116.3% and 0.01~7.16%, respectively. The method was validated and confirmed by quantification of the quality assurance samples of Industrial Safety and Health Research Institute, Korea Occupational Safety and Health Agency.