• 분석과학
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• 제30권2호
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• pp.102-111
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• 2017

Here we reported a methodology for identification of triacylglycerols (TAGs) and diacylglycerols (DAGs) in coix seed by preparative thin layer chromatography (prep-TLC) and non-aqueous reversed-phase liquid chromatography (NARP LC)-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS/MS). Lipid components were extracted from coix seed by reflux extraction using n-hexane for 3 hr. TAGs and DAGs in coix seed extract were effectively purified and isolated from matrix interferences by prep-TLC and then analyzed by LC-APCI-MS and MS/MS for identification. TAGs were effectively identified taking into consideration of their LC retention behavior, APCI-MS spectra patterns, and MS/MS spectra of $[DAG]^+$ ions. In MS/MS spectra of TAGs, diacylglycerol-like fragment $[DAG]^+$ ions were useful to identify TAGs with isobaric fragment ions. Based on an established method, 27 TAGs and 8 DAGs were identified in coix seed extract. Among them, 15 TAGs and 8 DAGs were for the first time observed in coix seed. Interestingly, some of TAGs isolated by prep-TLC were partly converted into DAGs through probably photolysis process during storing in room temperature. Thus, degradation phenomenon of TAGs should be considered in the quality evaluation and nutritional property of coix seed. LC-APCI-MS/MS combined with prep-TLC will be practical method for precise TAG and DAG analysis of other herbal plants.

• 생약학회지
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• 제44권4호
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• pp.350-361
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• 2013

Asarum sieboldii has been used for treatment of fever, pain, common cold, and chronic sinusitis in Korea. In this study, we performed quantification analysis of seven major constituents including aristolochic acid I, aristolochic acid II, ${\alpha}$-asarone, ${\beta}$-asarone, elemicin, methyl eugenol, and safrole in the 70% ethanol extract of Asarum sieboldii and its solvent fractions, n-hexane, ethylacetate, n-butanol, and water ones using a ultra-performance liquid chromatography-electrospray ionization-mass spectrometer(UPLC-ESI-MS) and gas chromatography-mass spectrometer(GC-MS). Regression equations of seven components were acquired with $r^2$ values >0.99. The values of limit of detection(LOD) and quantification(LOQ) were 0.1-3.9 ng/mL and 0.3-11.7 mg/mL, respectively. The amount of the seven compounds in Asarum sieboldii were not detected -143.66 mg/g. The established LC-MS/MS and GC-MS methods will be helpful to improve quality control of Asarum sieboldii.

• Journal of Microbiology
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• 제42권3호
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• pp.200-204
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• 2004

Retron is a prokaryotic genetic element that produces multicopy single-stranded DNA covalently linked to RNA (msDNA) by a reverse transcriptase. It was found that cells producing a large amount of msDNA, rather than those that did not, showed a higher rate of mutation. In order to understand the molecular mechanism connecting msDNA production to the high mutation rate the protein patterns were compared by two dimensional gel electrophoresis. Ten proteins were found to be differentially expressed at levels more than three fold greater in cells with than without msDNA, nine of which were identified by MALDI TOF MS. Eight of the nine identified proteins were repressed in msDNA-producing cells and, surprisingly, most were proteins functioning in the dissimilation of various carbon sources. One protein was induced four fold greater in the msDNA producing cells and was identified as a 30S ribosomal protein S2 involved in the regulation of translation. The molecular mechanism underlying the elevated mutation in msDNA-producing cell still remains elusive.

• 한국연초학회지
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• 제29권2호
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• pp.132-139
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• 2007

This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

• 식물조직배양학회지
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• 제22권6호
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• pp.307-310
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• 1995

Pelargonium aridum과 P. zonale의 자엽과 유식물의 절편체를 2 mg/L NAA와 0.2 mg/L BA를 첨가한 MS배지에서 배양하였을 때 캘러스를 형성하였다. 이들 캘러스는 동일배지에서 계대배양양하였다. 계대배양된 캘러스는 P. aridum의 경우 0.1∼l mg/L NAA와 0.25∼2 mg/L BA에서, P. zonale의 경우 0.1∼0.5 mg/L NAA와 1∼2 mg/L BA를 첨가한 MS 배지에 옮겨주었을 때 가장 많은 shoot를 형성하였다(P. aridum은 explant당 0.78개, P.zonale은 0.65개). 대부분의 shoot은 1/2 MS기본배지에서 배양하였을 때 발근하였다. 이들 재분화 개체들은 화분으로 옮겨진 추 온실에서 발육하여 개화하였다

• 한국자기공명학회논문지
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• 제22권2호
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• pp.26-33
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• 2018

Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.

• Mass Spectrometry Letters
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• 제2권3호
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• pp.69-72
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• 2011

Defective synthesis of the steroid hormones by the adrenal cortex has profound effects on human development and homeostasis. Due to the time-consuming chromatography procedure combined with mass spectrometry, the matrix-assisted laser desorption ionization method coupled to the linear ion-trap tandem mass spectrometry (MALDI-LTQ-MS/MS) was developed for quantitative analysis of 10 adrenal steroids in human serum. Although MALDI-MS can be introduced for its applicability as a high-throughput screening method, it has a limitation on reproducibility within and between samples, which renders poor reproducibility for quantification. For quantitative MALDI-MS/MS analysis, the stable-isotope labeled internal standards were used and the conditions of crystallization were tested. The precision and accuracy were 3.1~35.5% and 83.8~138.5%, respectively, when a mixture of 10 mg/mL ${\alpha}$-cyano-4-hydroxycinnamic acid in 0.2% TFA of 70% acetonitrile was used as the MALDI matrix. The limit of quantification ranged from 5 to 340 ng/mL, and the linearity as a correlation coefficient was higher than 0.988 for all analytes in the calibration range. Clinical applications include quantitative analyses of patients with congenital adrenal hyperplasia. The devised MALDI-MS/MS technique could be successfully applied to diagnosis of clinical samples.

• Journal of Plant Biotechnology
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• 제32권4호
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• pp.281-285
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• 2005

우리나라 자생식물인 산호수 (Ardisia pusilla DC)를 기내에서 대량증식하기 위하여 초대배양으로 산호수 경정을 MS, 1/2MS 배지에 BA와 TDZ의 농도를 달리하여 첨가된 배지에 치상하여 배양하였다. 무기염류를 달리한 배지와 생장조절물질 농도를 다르게 한 배지 중 1/2MS 배지에 BA 0.5mL가 첨가된 배지가 신초 수 7개 이상으로 증식이 양호하여 산호수의 초대배양에 적정배지로 나타났다. TDZ를 첨가한 배지에서는 캘러스형성이 과다하여 부정아 형성을 오히려 방해하여 BA 첨가배지보다 신초증식이 양호하지 못하였다. 신초의 증식을 위해 1/2 MS 배지에 BA 0.5 mg와 sucrose의 농도를 달리하여 첨가한 결과, sucrose 농도 20 g/L를 첨가한 배지에서 신초의 증식, 생장 및 다아체 형성이 양호하였다. 형성된 신초의 발근은 1/2MS 배지에 IBA, NAA를 각각 첨가한 배지를 사용하였는데 두 가지 옥신류에서 0.5 mg의 농도에서 신초의 생장과 발근이 양호하였다. 잎과 뿌리가 잘 발달한 유식물체를 원예용 상토에 옮겨 키웠을 때 모든 개체가 정상적인 형태로 성장하였다.

• 분석과학
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• 제23권5호
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• pp.457-464
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• 2010

먹는물(정수) 중에 잔류하는 버지니아마이신을 비롯한 macrolide 계열 의약물질 3종과 시메티딘을 동시에 정량 및 정성 분석하는 방법을 확립하였다. HLB 카트리지를 사용하여 분석물질을 추출/정제 및 농축한 후, HPLC/ESI-MS/MS를 이용하여 4종의 물질들을 효과적으로 분리하고 감도 좋게 검출할 수 있었다. 정량분석을 위해서 0.01~2.0 ng/mL 범위에서 $r^2$=0.995이상의 높은 직선성을 나타내는 검량선을 얻었으며, 시메티딘(37.7~48.1%)을 제외한 macrolide 계열 3종 의약물질은 64.7~118.1% 범위의 양호한 회수율을 나타내었다. 바탕 정수에 소량 첨가하여 얻은 분석방법의 검출한계와 정량한계는 각각 1.6~74.8 pg/mL 와 5.5~249.7 pg/mL 범위의 높은 감도를 나타내었다.

• 한국동물위생학회지
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• 제42권3호
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• pp.127-133
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• 2019

The purpose of this study was to investigate the contamination level of representative mycotoxins that have adverse effects on livestock by using LC-MS/MS method and to utilize the results as basic data for the establishment of quality control system for feed, and to provide information on production and storage. A total of nine mycotoxins, including aflatoxin $B_1$, aflatoxin $B_2$, aflatoxin $G_1$, aflatoxin $G_2$, ochratoxin A, fumonisin $B_1$, fumonisin $B_2$, deoxynivalenol (DON), zearalenone (ZEN) were simultaneously analyzed in LC-MS/MS under ESI positive mode. Fumonisin $B_1$ and fumonisin $B_2$ were detected from 3 cases of 75 forage produced in Incheon area, the detection rate was 4.0%. The detection concentration was 0.01~0.02 mg/kg, which was lower than the domestic recommended limit. Fumonisins were detected in a slightly different manner from the results of mycotoxin studies reported in Korea, which is attributed to the high temperature and dry summer weather of the year. The result of LC-MS/MS method performance of 9 mycotoxins, the recovery of DON was quite low as $41.53{\pm}3.91%$ that is not suitable for simultaneous analysis. This is probably due to that the extract solution used in this study was not suitable for the extraction of DON, along with the characteristics of a very dry forage. For the study of mycotoxins in Incheon area forage for the first time, further investigation is needed for the safe supply of livestock products.