• Mass Spectrometry Letters
• /
• 제2권1호
• /
• pp.16-19
• /
• 2011

Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

• 약학회지
• /
• 제32권1호
• /
• pp.50-54
• /
• 1988

A simple and sensitive method was studied for the simultaneous determination of catecholamine, indoleamine and their related metabolites by high performance liquid chromatography with electrochemical detector. Norepinephrine, dopamine, serotonin and their metabolites of 3,4-dihydroxyphenylacetic acid, homovanillic acid, 5-indoleacetic acid were resolved from rat brain tissue homogenates by separation on reversed phase $C_{18}$ column with mobile phase consisting of monochloroacetate buffer (pH2.47), 1.42mM sodium octyl sulfonate and 7% acetonitrile. Both catechols and indoles can be eluted in 15min. The sensitivities of this method are sufficient for determination of at least 100 pg of neurochemical amines in brain samples, for example, frontal cortex, olfactory bulb, striatum, septum, hippocampus, thalamus, hypothalamus, medulla & pons and cerebellum. The highest level of dopamine was observed in striatum whereas norepinephrine and serotonin were in hypothalamus.

• Archives of Pharmacal Research
• /
• 제27권1호
• /
• pp.35-39
• /
• 2004

The method for the chiral analysis of (-)-yatein was developed and the distribution of this component in the plants of three genera like Juniperus, Thuja and Chamaecyparis belonging to Cupressaceae family was examined. The chiral analysis of (-)-yatein from the plants was carried out by high performance liquid chromatography on (R,R)-Whelk-O1 column using 81 v/v% methanol as mobile phase. The yatein content in the leaves of Juniperus was the highest in compare with that of the other two genera, providing the possibility of the chemical discrimination of the plants in Juniperus from the other plants in the Cupressaceae family. In general, the yatein content in the leaves was much higher than that in the twigs. This method could be applied for the quality control of (-)-yatein in the plants belonging to Cupressaceae family.

• 분석과학
• /
• 제19권6호
• /
• pp.519-528
• /
• 2006

본 연구에서는 뇨시료를 고체상 추출법으로 추출한 후 HPLC/DAD/ESI-MS(high-performance liquid chromatograph/diode array detector/electro-spray ionitation mass spectrometry)를 사용하여 분석하였다. 7종의 thyroid hormones의 HPLC 분리조건은 Hypersil ODS(octadecylsilica) 컬럼(4.6mm I.D., 100 mm length, particle size $5{\mu}m$)을 사용하고 ammonium formate buffer와 acetonitrile을 이동상으로 하여 기울기 용리한 결과 완전 분리가 가능하였으며, UV spectra 및 질량스펙트럼을 확인할 수 있었다. 고체상 추출법에 의한 전처리 최적 조건을 조사한 결과 시료를 pH 3으로 한 후 C18 고체상을 사용하여 4 mL의 methanol/ammonium hydroxide(9:1) 혼합용액으로 용리할 경우 회수율이 89.0-113.1%로 나타났다. HPLC/DAD를 이용하여 10-1000 ng/mL범위에서 검량선을 작성한 결과 $r^2$값은 0.992-0.998 으로 나타났으며 검출한계는 2-4 ng/mL(3.8-13.0 pmol/mL)로 계산되었다.

• 분석과학
• /
• 제27권3호
• /
• pp.140-146
• /
• 2014

후 컬럼 동위원소 희석법(PCID, post column isotope dilution)을 HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry)에 적용한 정량법에서 내부 표준물을 동시에 사용하여 정확도와 정밀도를 개선하였다. 전통적인 여러 정량법과 후 컬럼 동위원소 희석법을 비교하여 볼 때에 PCID의 경우에 컬럼내에서 발생하는 오차가 가장 큰 요인으로 작용하였음을 알 수 있었다. PCID에서 내부 표준물을 사용하여 컬럼내에서의 손실에 대한 오차를 효과적으로 보정하고 정확도와 정밀도를 개선할 수 있었다. 셀레늄 화학종인 SeMet을 시료로 사용하고 내부 표준물로 MeSecys 또는 $Se^{4+}$를 이용한 결과, 사용하지 않은 경우와 비교하면 상대오차는 각 각 31%와 13%에서 모두 1% 대로 낮아져 정확도가 크게 개선되었으며, 상대 표준편차는 5.1%와 6.9%에서 각각 1.5%와 0.2%로 정밀도 또한 크게 개선되었다. PCID에서 내부 표준물을 사용하였을 때의 정량분석법의 장점을 다른 분석법과 비교 토의하였다.

• 대한한의학회지
• /
• 제25권3호
• /
• pp.45-54
• /
• 2004

Objectives : This study was aimed to evaluate marker substances in Gami-Honghwa-Tang (KH-19) by high performance liquid chromatography-photodiode array detector (HPLC-DAD). Gami-Honghwa-Tang is composed of nine crude herbs, Rehmanniae Radix Preparata, Angelicae Gigantis Radix, Cnidii Rhizoma, Paeoniae Radix, Corni Fructus, Moutan Cortex Radicis, Lycii Fructus, Carthami Flos and Glycyrrhizae Radix. Methods : The separation was performed on an Aquasil C18 (4.6×250mm) column by gradient elution with 0.05% TFA in H2O - 0.05% TFA in acetonitrile (0 min 100:0, 20 min 90:10, 40 min 70:30, 60 min 50:50, 80 min 0:100, 90 min 100:0) as the mobile phase at a flow-rate of 1.0 ml/min with detection at 190-800nm. Also we examined the contents for bacteria, pesticide residue and harmful heavy metals. Results : HPLC-DAD was employed to determine the quantities and the qualities of several marker substances such as 5­hydroxymethyl-2-furaldehyde (5-HMF), paeonol, loganin, paeoniflorin, glycyrrhizin, and decursin in the KH-19. There were no bacterial contents, pesticide residues, or harmful heavy metals. Conclusions : We suggest these results could be a useful evidence for quality control of KH-19. This method permits fingerprints of selected individual marker substances from herbal prescriptions without derivatization, multiple purification steps, or lengthy separation times.

• 대한약침학회지
• /
• 제18권1호
• /
• pp.44-55
• /
• 2015

Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes.

• 한국자원식물학회지
• /
• 제9권1호
• /
• pp.47-54
• /
• 1996

할미꽃의 뿌리에 함유되어 있는 제초활성물질의 확인과 동정을 위하여 이들을 추출 정제하고 활성성분 및 제초활성을 조사하여 다음과 같은 결과를 얻었다. 1. 각종 칼럼크로마토그래피법과 Prep. HPLC의 순차적인 적용에 의해 제초활성물질이 포함된 할미꽃 뿌리의 메타놀추출물을 정제하여 2개의 활성분획을 획득하였다. 2. 최종적으로 얻어진 활성분획들을 100ppm의 농도로 조제하여 처리한 결과, 식용피 유근의 생장 억제율은 대조구에 비해 각각 48% 및 60%로 나타났다. 3. GC-MS Spectrometry에 의해 분리된 활성분획 중의 성분들을 기존자료들과 비교하여 수종의 지방산 에스테르, 2종의 탄화수소류, squalene, evidonol 및 1종의 diazepin 관련 화합물이 동정되었다.

• 대한한의학회지
• /
• 제32권4호
• /
• pp.68-74
• /
• 2011

Objective: The purpose of this study is to expatiate on high performance thin layer chromatography (HPTLC) as a simple, easy and scientific method for evaluation and standardization of herbal formulae. Methods: Through retrieving HPTLC application for herbal formulae in the literatures, the current situation of HPTLC application, and potential as well as limitation of HPTLC as a standardization method for multi-herbal drug was studied. Results: HPTLC is a speedy, inexpensive and well-operable tool for possessing multi-capability on component identification, separation, quantification and purification compared to other methods, such as high performance liquid chromatography (HPLC), gas chromatography (GC). Conclusions: HPTLC is considered as an available and convenient method for quality control and standardization of multi-herbal drugs. Thereby, this method could be recommended to widely applicate in the traditional Korean medicine.

• Bulletin of the Korean Chemical Society
• /
• 제34권12호
• /
• pp.3629-3634
• /
• 2013

In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.