• Journal of Applied Biological Chemistry
• /
• 제66권
• /
• pp.338-344
• /
• 2023

Curcuma longa is a plant belonging to the genus Curcuma and is distributed across various Asian regions. This plant is widely known for its rhizomes, which possess a variety of pharmacological properties. However, although the leaves and stems of this plant also contain several health-promoting secondary metabolites, very few studies have characterized these compounds. Therefore, our study sought to quantify the secondary metabolites from the leaves and stems of Curcuma longa L. (LSCL) using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) and high-performance liquid chromatography (HPLC). Our LC-ESI-MS analyses detected twenty-one phenolic compounds in the LSCL, among which fifteen compounds were detected via HPLC analysis. Four compounds, namely vanillic acid (0.129 mg/g), p-coumaric acid (0.431 mg/g), 4-methylcatechol (0.199 mg/g), and afzelin (0.074 mg/g) were then quantified. These findings suggest that LSCL is rich in secondary metabolites and holds potential as a valuable resource for the development of functional and nutritional supplements in the future.

• 대한화장품학회지
• /
• 제25권3호
• /
• pp.23-46
• /
• 1999

LC/MS는 HPLC의 분리능과 질량분석기의 화합물의 확인 능력을 결합시킨 기기이다. 여기서 사용되는 이온화 방법은 GCJMS에서 사용되어지는 전자이온화법(electron ionization, EI)이나, 화학이온화법(chemical ionization, CI)은 부적당하기 때문에 최근 개발되어진 연성 이온화법의 대표적인 고속원자폭격식(Fast atom bombardment, FAB)이나 전기분무이온화식 (electrospray ionization, ESI) 등이 사용되고 있다. 이중 전기분무이온화법은 고속원자폭격법에서 사용되는 매트릭스를 사용하지 않기 때문에 매트릭스 이온의 부재로 인한 낮은 바탕 신호, 오래 지속되면서 안정된 초기 이온 전류, 샘플링의 용이성, HPLC와의 더 좋은 호환성 등의 장점을 제공한다. 이러한 전기분무이온화 방법은 극성이 매우 크거나 휘발성이 낮은 물질로 보통의 EI나 CI 이온화 방법으로 분석이 어려운 물질들을 분석할 수 있다. 또한 열에 불안정하거나 분자의 분자량이 다른 단백질 등의 분석도 가능하다. 이러한 LC/ESI/MS 방법을 이용하여 열에 불안정하고 극성이면서 분자량이 커서 GC/MS 펄의 분석이 어려운 기능성 화장품 원료로 주목받고 있고 생체에 존재하는 지질 성분으로 알려진 레시틴과 세라마이드의 분석이 가능함을 소개하고 분리와 동시에 그 분자량과 구조에 대한 정보를 빠르게 얻을 수 있음을 소개하였다.

• Bulletin of the Korean Chemical Society
• /
• 제17권11호
• /
• pp.1036-1039
• /
• 1996

Synthetic lipoidal peptides based on viral protein sequences have been prepared. These peptides contain an N-palmitoyl group at the N-terminal residue, which is a modified cysteine, containing a S-[2,3-bis(acyloxy)-(2-R,S)-propyl] moiety. When this residue (Pam3Cys) is at the N-terminus of a synthetic peptide, it acts as potent immunoadjuvant to enhance both IgM and IgG antibody responses to the attached peptide. Conventional analytical procedures (e.g., Edman degradation and amino acid analysis) are either not applicable due to the N-terminal modification, or do not provide confirmation of the intact structure. Chromatographic analysis is also hindered by the tendency of these lipoidal Pam3Cys peptides to form large aggregates, and in some cases to be permanently adsorbed on reversed phase columns. We have applied several mass spectrometric techniques, including fast atom bombardment (FAB), electrospray ionization (ESI) and matrix assisted laser desorption ionization (MALDI) to characterize the intact structures of a number of different Pam3Cys synthetic peptides. The MALDI-MS has been found to be the most sensitive for the analysis of the structure of Pam3Cys peptides.

• Mass Spectrometry Letters
• /
• 제12권3호
• /
• pp.118-124
• /
• 2021

Many previous studies have focused on revealing the harmfulness of microplastic particles, whereas very few studies have focused on the effects of chemicals, particularly photooxidation product. In this study, products of photodegradation from expanded polystyrene (EPS), compounds produced by photolysis by ultraviolet (UV) light, were investigated. EPS was directly irradiated and photolyzed using a UV lamp, and then the extracted sample was analyzed using high-resolution mass spectrometry (HRMS). Multiple ionization techniques, including electrospray ionization, atmospheric pressure chemical ionization, and atmospheric pressure photoionization, were used. In total, >300 compounds were observed, among which polystyrene monomer, dimer, and oxidized products were observed. In this work, the data presented clearly demonstrate that it is necessary to identify and monitor oxidized plastic compounds and assess their effect on the environment.

• Mass Spectrometry Letters
• /
• 제3권3호
• /
• pp.82-85
• /
• 2012

The formation of zinc finger peptide-$Zn^{2+}$ complexes in electrospray ionization mass spectrometry (ESI-MS) was examined using three different metal ion sources: $ZnCl_2$, $Zn(CH_3COO)_2$, and $Zn(OOC(CHOH)_2COO)$. For the four zinc finger peptides (Sp1-1, Sp1-3, CF2II-4, and CF2II-6) that bind only a single $Zn^{2+}$ in the native condition, electrospray of apo-zinc finger in solution containing $ZnCl_2$ or $Zn(CH_3COO)_2$ resulted in the formation of zinc finger-$Zn^{2+}$ complexes with multiple zinc ions. This result suggests the formation of nonspecific zinc finger-$Zn^{2+}$ complexes. Zn(tartrate), $Zn(OOC(CHOH)_2COO)$, mainly produced specific zinc finger-$Zn^{2+}$ complexes with a single zinc ion. This study clearly indicates that tartrate is an excellent counter ion in ESI-MS studies of zinc finger-$Zn^{2+}$ complexes, which prevents the formation of nonspecific zinc finger-$Zn^{2+}$ complexes.

• Food Science and Biotechnology
• /
• 제18권1호
• /
• pp.113-117
• /
• 2009

A method was developed using enhanced liquid chromatography coupled with electrospray ionization mass spectrometry for the analysis and quantitation of 2 main potato glycoalkaloids, $\alpha$-chaconine, and $\alpha$-solanine, without any pre-concentration or derivatisation steps. Calibration curves generated by this technique exhibited a linear dynamic range from 0.025 to $50{\mu}g/mL$ and from 0.05 to $50{\mu}g/mL$ for $\alpha$-chaconine and $\alpha$-solanine, respectively. Matrix effects were evaluated by comparing calibration curves measured in matrix-matched and solvent-based systems. Ion suppression due to matrix effects was weak and extraction recoveries of 88 to 114% were obtained in different sample matrices spiked with analyte concentrations ranging from 15 to $35{\mu}g/mL$. Potatoes that had been genetically modified to tolerate glufosinate contained the same glycoalkaloid levels as their non-transgenic counterpart. We suggest complementing compositional comparison assessment strategy by validating quantitative analytical methods for the toxic glycoalkaloids in potato plants.

• Mass Spectrometry Letters
• /
• 제3권4호
• /
• pp.87-92
• /
• 2012

In this study, we explored a new approach for generating ions of organics and biomolecules using contactless atmospheric pressure ionization (C-API). That is, a tapered capillary (~20 cm) was connected to a syringe, which was coupled to a syringe pump for providing a given flow rate to introduce sample solution to the proximity of a mass spectrometer. The gas phase ions derived from analytes were readily formed in the capillary outlet, which was very close to the mass spectrometer (~1 mm). No external electric connection was applied on the capillary emitter. This setup is very simple, but it can function as an ion source. This approach can be readily used for the analysis of small molecules such as amino acids and large molecules such as peptides and proteins. The limit of the detection of this approach was estimated to be ~10 pM when using bradykinin as the sample. Thus, we believe that this approach should be very useful for being used as an alternative ion source because of its low cost, high sensitivity, simplicity, and ease of operation.

• Mass Spectrometry Letters
• /
• 제4권4호
• /
• pp.83-86
• /
• 2013

A new interface for coupling CIEF and MS using a four-way cross has been developed in a single mechanical system. This new interface could be operated without the electric discontinuity and reinstallation of lines. Additionally, a bare fused silica capillary was facilitated as a spray needle to produce electrospray and to guide catholyte or sheath liquid. Focusing for CIEF was completed in a hanging droplet at the end of spray needle. This capillary spray needle also provided stable spray, enhanced the ionization efficiency and increased sensitivity. Results with carbonic anhydrase I showed that focusing and spraying were well completed with the new interface and the new spray needle.

• Fibers and Polymers
• /
• 제3권4호
• /
• pp.140-146
• /
• 2002

Non-genotoxic diamines 2,2'-dimethyl-5,5'-dipropoxybenzidine and 5,5'-dipropoxy-benzidine were employed as potential alternatives to benzidine in the synthesis and evaluation of new direct dyes for cotton. Assessment of the resultant dyes indicated that both diamines can be used to prepare new direct dyes having colors and fastness properties that make them comparable to commercial direct dyes, and that the structures of the new direct dyes can be confirmed by negative ion electrospray mass spectrometry (ESMS). The mutagenic properties of new direct dyes were established using the standard Ames Salmonella mammalian mutagenicity assay.

• 분석과학
• /
• 제17권3호
• /
• pp.263-270
• /
• 2004

알킬페놀에톡실레이트 (APEO)는 주로 비이온성 계면활성제로 쓰이고 있으며 세제, 액체연료 및 농약에도 이용이 되고 있다. APEO 자체는 독성물질로 분류되어 있지 않지만, 그 대사생성물질인 단사슬 APEO, 알킬페놀 및 카르복실 유도체등은 폐수 또는 음용수를 염소처리하는 동안 mutagenic ring halogenated derivative를 생성한다. 이들 생성물들은 estrogenic effect를 나타내기 때문에 APEO를 제한 또는 규제하고 있는 추세이다. 본 연구에서는 APEO의 대사체로서 단사슬 APEO 인 4-nonylphenol-di-ethoxylate (NP2EO), 4-octylphenol-di-ethoxylate (OP2EO)를 분석하기 위해서 p-n-nonylphenol-di-ethoxylate-ring-$^{13}C_6$을 내부표준물질로 사용하여 HPLC/ESI/MS를 이용하여 분석하였다. 분석조건은 이온화 용매인 trifluoroacetic acid가 $10{\mu}M$이 되도록 각각 물과 메탄올에 첨가시켜 사용하였다. 물시료 1 L에 진한 황산을 이용하여 pH를 2이하로 조정한 후, 아세톤, 메탄올 및 물 (pH 2)로 활성화시킨 Sep-Pak $C_{18}$에 loading 시킨 후 아세톤으로 용출하여 시료용액으로 하였다. 이 방법으로 농도범위가 20 ~ 500 ng/L 내에서 검량선의 직선성은 r=0.999 (OP2EO)와 0.990 (NP2EO)였으며, 검출한계는 OP2EO는 20 ng/L, NP2EO는 50 ng/L 이었다. 정확도 및 정밀도는 85.8~122.1% 및 8.2~18.8 %로 좋은 결과를 나타냈다. 이 방법은 환경시료로부터 미량의 APEO를 분석하는데 사용될 수 있고, APEO 오염실태 조사에 응용될 수 있을 것으로 사료된다.