• 분석과학
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• 제28권2호
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• pp.79-85
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• 2015

TLC (SiO₂) 상에서 3가지 유사 암페타민 류 아민 화합물과 3가지 유도체화 시약 사이의 반응으로부터 얻어진 아민유도체의 이미지 분석으로부터 암페타민 류 화합물에 대한 신속하고 경제적인 반정량적인 분석방법을 제시하기 위하여 선행 실험을 하였다. TLC상 직접적인(in situ, co-spot) 유도체화 반응의 적정화를 시도하였고 그 TLC 결과물들을 디지털카메라로 촬영하여 이미지를 얻은 후 2가지의 이미지 분석 프로그램(CP Atlas 2.0 및 ImageJ)에 적용하여 재현성(RSD; %)과 상관성(R²)을 각각 확인 및 비교하였다. 그 결과, 반응 조건에 대한 조정이 필요하였고(반응 온도 등) 각 시료별 2가지의 농도(0.5 mg/mL 및 0.01 mg/mL)에서 반응의 재현성은 0.69~5.50% 범위이었으며 반응(2 µL per spot)의 생성물과 아민의 농도에 대한 상관성은 0.1~0.005 mg/mL의 농도 구간에서 가장 높게 나타났다(R²> 0.9906). 또한, 두 가지 프로그램 모두 재현성과 직선성에 대한 유사한 결과를 나타내어 직접적인 유도체화 반응과 TLC 이미지에 대한 이들 프로그램을 사용한 분석이 아민 화합물에 대한 반정량적인 분석으로 사용될 수 있는 가능성을 보였다.

• 대한수의학회지
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• 제44권1호
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• pp.23-28
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• 2004

We established a new method to analyze moxidectin using high performance liquid chromatography(HPLC) with fluorescence derivatization in order to obtain its residual profiles in biological samples. Recovery of moxidectin in tissue was 62% at 10 ppb. Average detection reproducibility in terms of coefficience variation was 4.47% at 0.32 to 10 ppb. Residual of moxidectin was studied in 44 Yorkshire-Landrace mixed bred male pigs administered subcutaneously 0, 200, or $800{\mu}g/kg$ body weight (BW) Residual profiles of moxdectin in blood, muscle, liver, kidney and fat of pigs were described. The concentration of the moxidectin in liver after administration of moxidectin was the highest among the tissues examined. Moxidectin in liver after administration of moxidectin as $200{\mu}g/kg$ BW was declined from $10.0{\pm}3.7ng/g$ at 10 day post administration to $0.5{\pm}0.3ng/g$ level at 40 day post administration. Residual levels of moxidectin in all samples were estimated to fall below the limit of quantitation (0.32 ng/ml) after 50 day after treatment of $200{\mu}g/kg$. Moxidectin showed no abnormal observations in all the clinical findings at any concentrations under these experimental conditions. In conclusion, this analysis method by HPLC after fluorescence derivatization was very effective for the detection of moxidectin in biological samples. We suggest that 50-day is safe enough for the withdrawal time of moxidectin in pigs, following the recommendation dose by the manufacturer.

• 약학회지
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• 제59권1호
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• pp.6-11
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• 2015

A simple HPLC-UV method was developed and validated for the quantification of human serum isepamicin using phenylisocyanate as a derivatization agent. The linear calibration curve was obtained in the concentration range of $1{\sim}100{\mu}g/ml$ and LLOQ of $1{\mu}g/ml$. This method was validated with selectivity, linearity, precision and accuracy, leading to successful application for estimating the pharmacokinetic parameters of isepamicin in Korean healthy subjects following IV infusion of 800 mg isepamicin. The mean $t_{1/2}$ of isepamicin was $1.55{\pm}0.08hr$.

• 분석과학
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• 제33권1호
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• pp.23-32
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• 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.

• 한국환경농학회지
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• 제41권3호
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• pp.206-216
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• 2022

BACKGROUND: Dithiocarbamate fungicide propineb can be analyzed quantitatively by derivatization reaction followed by HPLC/UVD, which has high reproducibility and stability. However, the presence of high protein in soybeans and peas affects the derivatization process resulting in extremely low recoveries. Therefore, this study was conducted to improve the analytical method for analysis of propineb in soybeans and peas by applying a deproteinization process using chloroform-gel method. METHODS AND RESULTS: The deproteinization process was carried out up to 6 times for soybeans and 5 times for peas using 50 mL chloroform. After 4 times of deproteinization process followed by a derivatization reaction with methyl iodide, the recovery yields of propineb in both pulses were >90%. However, the recovery yield tended to decrease when the deproteinization process was performed more than 5 times. The method limit of quantification (LOQ) was 0.04 mg/L. The recovery conducted in triplicate at 10 times and 50 times of the LOQ ranged from 87.2 to 95.0 % with a coefficient of variation <10%. CONCLUSION(S): This study confirmed that 4 times of deproteinization process using the chloroform-gel method was effective when derivatizing and analyzing dithiocarbamate fungicides in pulses with high protein content. However, depending on the initial protein content present in the pulses, there was a difference in the recovery: the lower the protein content, the higher the recovery rate of propineb. It is expected that the method proposed in this study could be applied to remove high content of protein as analytical interference substance from agricultural samples.

• 한국식품위생안전성학회지
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• 제11권2호
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• pp.149-157
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• 1996

A procedure for the determination of Aflatoxins in food and grains which utilizes reversed phased liquid chromatographic (LC) analysis with postcolumn derivatization by an electrochemical cell and determination with a fluorescence detector has been evaluated. The LC mobile phase was water-acetonitrile-methanol (6+2+2) with 1mM KBr and 1 mM HNO3 which gave baseline separation for the four Aflatoxins (AfB1, AfB2, AfG1, AfG2). The electrochemical cell set at 7V, generated bromine and derivatized aflatoxins B1 and G1, The derivatives were detected by the fluorescence detector. The aflatoxins in naturally contaminated corn samples were isolated by three different cleanup procedures: the AOAC method I column(CB method), a rapid filtrate column (Romer's column), and an immunoaffinity column. The final extract were quantitated with fluordensitometric TLC and the LC postcolumn derivatization techniques. The results were quite similar, however the LC technique showed less interferences and could be automated. Samples of corn, raw peanuts, peanut butter and dried dates were also analyzed successfully with this procedure.

• 한국표면공학회지
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• 제32권3호
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• pp.344-350
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• 1999

The surface chemical structure of three kinds of polyethylene (PE): high density (HD) PE, low density (LD) PE and linear (L)-LDPE exposed to Ar and $O_2$ plasmas has been investigated using XPS. Oxygen was incorporated in a more increased amount for HDPE than for L-LDPE and LDPE. Ar plasma tended to incorporate more oxygen than $O_2$ plasma. The XPS valence band spectra for Ar plasma exhibited a clear peak assigned to $O_2$s character. By chemical derivatization method it was found that the amount of -COOH group at the surface was much greater than that of -OH group. The hydrophilic nature of plasma-treated PE increased in the order: LDPE

• Mass Spectrometry Letters
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• 제11권4호
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• pp.103-107
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• 2020

We report the application of 2,4,6-trichlorobenzoyl chloride (often referred to as Yamaguchi esterification reagent) for the selective derivatization of the carboxylic group for GC-MS with the sample preparation method optimized for GC-MS analysis. The reagent was shown to be capable of selectively turning the carboxylic group into a reaction center, i.e., anhydride, of which the further reaction was directed to a near complete formation of required esters by unique steric and electronic effects of the reagent. Using the developed method, the chiral separation of hydroxycarboxylic acids by GC-MS using non-chiral columns was successfully demonstrated.

• Biomolecules & Therapeutics
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• 제31권5호
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• pp.566-572
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• 2023

A chiral derivatization strategy with phenylglycine methyl ester (PGME) was employed to develop a straightforward method to determine the absolute configurations of N,N-dimethyl amino acids. The PGME derivatives were analyzed using liquid chromatography-mass spectrometry to identify the absolute configurations of various N,N-dimethyl amino acids based on their elution time and order. The established method was applied to assign the absolute configuration of the N,N-dimethyl phenylalanine in sanjoinine A (4), a cyclopeptide alkaloid isolated from Zizyphi Spinosi Semen widely used as herbal medicine for insomnia. Sanjoinine A displayed production of nitric oxide (NO) in LPS-activated RAW 264.7 cells.

• 한국축산식품학회지
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• 제41권4호
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• pp.731-738
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• 2021

Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.