• 분석과학
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• 제36권5호
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• pp.250-257
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• 2023

The development of a spectrofluorimetric method for the determination of trimethoprim according to the reaction between O-phthalaldehyde (OPA) in highly alkaline media, and 2-mercaptoethanol (2ME) and this reaction gives fluorescent product measured at (458) nm when excited at (342) nm. The optimization of the analytical parameters that influence intensity was investigated. The intensity of fluorescence of the formed product was linearly related to the concentration of trimethoprim in the (100-1200) ng mL^-1 range. The limit of detection and limit of quantification were estimated to be (22.54) ng mL^-1 and (75.15) ng mL^-1 respectively. The utility of the proposed methods was successfully verified by analysis of trimethoprim in pure and real pharmaceutical preparations with high accuracy, the recovery percentages Re%, were found to be (100.5) % and (99.76) % for pure drug and pharmaceutical preparations respectively.

• Archives of Pharmacal Research
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• 제17권4호
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• pp.244-248
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• 1994

A stereoselective and sensitive high performance liquid chromatography using fluoresecence deterctor was examined for the determination of R(-) and S(+)-salbutamol in human plasma. Solid phase extraction method using silica as sorbent was used to extract salbutamol racemates from the plasma matrices. After fractionation and freeze-drying of the eluates containing salbutamol racemates, they were separated and quantified on a chirla stationary column. The detection limit of each enantiomer was 2 ng/ml in human plasma (S/N=3).

• 약학회지
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• 제23권1호
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• pp.7-10
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• 1979

A gas chromatographic determination of dienestrol in dienestrol cream has been studied. Dienestrol cream was dissolved in pyridine and silylation was done by using N, O-bis (trimethylsilyl) trifluoroacetamide. The derivative was injected into 3% silicone OV-17 column for chromatographic estimation. The dienestrol peak was found to be well separated from the other components of the cream. The detection limit was obtained to be $5.6{\times}10^{11}$ mol of dienestrol for this method. As there is no need for prior separation procedure, this experiment is extremely simple and less time consuming as compared to the conventional methods for estimation of dienestrol in cream.

• 한국환경보건학회지
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• 제32권1호
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• pp.67-70
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• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

• 생약학회지
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• 제51권3호
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• pp.207-216
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• 2020

The analysis method for qualitative analysis of the screening method that can be performed prior to the quantitative analysis of individual pesticide was reviewed in order to meet the safety standards that are being strengthened in the field of pesticide residue testing of herbal medicines. Among the residual pesticides presented in the Korean Pharmacopoeia, 56 pesticides, excluding 15 pesticides that need to be individually analyzed, were selected for analysis using QuEChERS preprocessing and GC-MS/MS, which are used in the existing agricultural products field. For each pesticide, the detection limit level of 0.001-0.005 mg/kg and the quantitative limit level of 0.002-0.017 mg/kg were confirmed. In the recovery test in which the standard was treated at a concentration of 0.02 mg/kg, it was confirmed that the proportion of pesticides satisfying the recovery of 70-120% was 85.7-96.4% for each herbal medicine, so it was confirmed that it was a level that could be reviewed by the screening method.

• Toxicological Research
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• 제35권2호
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• pp.161-165
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• 2019

Cysteamine has been used in cosmetics as an antioxidant, a hair straightening agent, and a hair waving agent. However, recent studies indicate that cysteamine can act as an allergen to hairdressers. The objective of this study was to develop and validate a simple and effective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the measurement of cysteamine and its dimer, cystamine. Sodium 1-heptanesulfonate (NaHpSO) was used as an ion-pairing agent to improve chromatographic performance. Separation was performed on a Gemini C18 column ($250mm{\times}4.6mm$, $5{\mu}m$ particle size) using a mobile phase composed of 85:15 (v/v) 4 mM NaHpSO in 0.1% phosphoric acid:acetonitrile. UV absorbance was monitored at 215 nm. The RP-HPLC method developed in this study was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, and recovery. Cysteamine and cystamine were chromatographically resolved from other reducing agents such as thioglycolic acid and cysteine. Extraction using water and chloroform resulted in the recovery for cysteamine and cystamine ranging from 100.2-102.7% and 90.6-98.7%, respectively. This validated RP-HPLC method would be useful for quality control and monitoring of cysteamine and cystamine in cosmetics.

• Natural Product Sciences
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• 제27권4호
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• pp.284-292
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• 2021

Recently, a phytoestrogenic functional food has been developed using the fruits of Sophora japonica. Phytochemical investigation of fruits of S. japonica led to the isolation of eight flavonoid glycosides using various chromatographic techniques. The isolated compounds were identified as genistin (1), sophoricoside (2), genistein 7,4'-di-O-β-D-glucopyransoide (3), sophorabioside (4), genistein-7-O-β-D-glucopyranoside-4'-O-[(α-L-rhamnopyranosyl)-(1→2)-β-D-glucopyranoside] (5), sophoraflavonoloside (6), nicotiflorin (7) and kaempferol-3-O-α-L-rhamnopyranosyl-(1→6)-β-D-glucopyranosyl-(1→3)-β-D-glucopyranoside (8), respectively, by comparison of their spectroscopic data with those reported in the literature. In addition, a new HPLC-DAD method for simultaneous determination of the isolated compounds was developed to quantitate the contents of flavonoids in S. japonica and S. flavescens. The method was validated in terms of limit of detection, limit of quantitation, specificity, linearity, precision and accuracy. The validated method was successfully applied to determine eight flavonoids in two Sophora species. The contents of eight flavonoids varied according to the parts and species. Particularly, it was found that only the fruits of S. japonica contained sophoricoside, a phytoestrogenic isoflavone.

• 한국식품과학회지
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• 제53권4호
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• pp.391-398
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• 2021

As global interest in herbal medicines has increased, the adulteration of herbal medicines has become a critical safety issue. Adulteration with dyes to improve the appearance of low-quality products is of particular concern. This study aimed to develop a high-performance liquid chromatography (HPLC) method to detect dyes added as adulterants to Phellodendron. Samples were analyzed on a C18 column using 50 mM ammonium acetate and acetonitrile as the mobile phase. All calibration curves showed good linearity (r² ≥0.9999) over the five-point concentration range (1-50 mg/kg). Limit of detection ranged from 0.04-0.35 mg/kg, and limit of quantification ranged from 0.11-1.07 mg/kg. The repeatability and reproducibility for these measurements were 94.2-103.3% and 96.6-103.8% for accuracy and 0.14-2.28 RSD (%) and 0.80-2.37 RSD (%) for precision. Moreover, the measurement uncertainty of the low, medium, and high concentrations for 10 dyes was considered. Thus, this HPLC method is suitable for detecting color adulteration of Phellodendron.

• 한국위성정보통신학회논문지
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• 제12권3호
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• pp.35-40
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• 2017

위성의 상태를 파악하기 위해 기존에는 OOL(Out-Of-Limit) 방식을 많이 사용하여 왔다. OOL은 특정 텔레메트리의 상위, 하위 문턱 값을 지정하여 해당 값을 벗어날 경우 문제가 발생한 것으로 인식 하는 방식이다. 이 방법은 파라미터의 특성을 파악하여 각각의 문턱 값을 정확히 설정해야 하는 전문 지식과 노력이 필요하고 텔레메트리 값이 문턱값 내에서 비정상적으로 변할 경우는 검출할 수 없다는 문제점이 있다. 이러한 문제를 극복하기 위해 본 논문에서는 위성이 정상 상태일 때 텔레메트리의 통계적 특징 중 러프집합을 이용하여 중요한 것을 선택, 적용하여 퍼지 모델을 구축하고 이상 상태를 구분하는 시스템을 제안한다. 정상 상태의 데이터만 이용하여 모델을 구축하기 때문에 출력값을 비교 하여 사전에 정의되지 않은 비정상 상태의 구분이 가능 하며 다양한 통계 값을 이용하기 때문에 전문 지식 필요 없이 문턱값 내에서 비정상적으로 변하는 텔레메트리를 검출할 수 있다. 제안한 시스템의 동작 확인을 위해 실제 저궤도 관측위성의 배터리 온도 텔레메트리를 적용하여 시험을 수행 하였고 비정규적 운영 상태에 대한 검출이 성공적으로 이루어 졌다.

• Journal of the Optical Society of Korea
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• 제20권6호
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• pp.669-677
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• 2016

A miniaturized FTIR spectrometer based on lamellar grating interferometry is being developed for passive remote-sensing. Consisting of a pair of micro-mirror arrays, the lamellar grating can be fabricated using MEMS technology. This paper describes a method to compute the optical field in the interferometer to optimize the design parameters of the lamellar grating FTIR spectrometer. The lower limit of the micro-mirror width in the grating is related to the formation of a Talbot image in the near field and is estimated to be about $100{\mu}m$ for the spectrometer to be used for the wavelength range of $7-14{\mu}m$. In calculating the far field at the detection window, the conventional Fraunhofer equation is inadequate for detection distance of our application, misleading the upper limit of the micro-mirror width to avoid interference from higher order diffractions. Instead, the far field is described by the unperturbed plane-wave combined with the boundary diffraction wave. As a result, the interference from the higher order diffractions turns out to be negligible as the micro-mirror width increases. Therefore, the upper limit of the micro-mirror width does not need to be set. Under this scheme, the interferometer patterns and their FT spectra are successfully generated.