• 분석과학
• /
• 제32권2호
• /
• pp.35-47
• /
• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• 한국식품저장유통학회지
• /
• 제30권2호
• /
• pp.235-246
• /
• 2023

Yellowball (Citrus hybrid cv. Yellowball ) is a new citrus hybrid between Haruka (C. tamurana × natsudaidai ) and Kiyomi (C. unshiu × sinensis) and is known to possess strong antioxidant activity. However, detailed information on the antioxidant components of its peel has not yet been reported. This study evaluated the antioxidant activity of the peel and identified the antioxidant components by fractionating a methanolic extract of Yellowball peels using liquid-liquid extraction with n-hexane, ethyl ether (ether), ethyl acetate (EA), butanol, and water. The phenolic contents and antioxidant activities of the n-hexane, ether, and EA fractions were higher than those of the other fractions, and these fractions were further separated by semi-preparative high-performance liquid chromatography (HPLC). Four antioxidant peaks, EA1, EA2, EA3, and He1, were isolated and analyzed using ultra-performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (UPLC-Q-TOF MS). Sinapoyl glucoside and hesperidin were identified in EA2 and EA3, respectively, and a polymethoxylated flavone (PMF) complex (5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, natsudaidain, tetrameth- oxyflavone, and tangeretin) was identified in He1. A compound in EA1 with m/z 223.0246 [M-H] could not be identified and was named unknown2. The antioxidant activity of unknown2 (IC₅₀=69.17 ㎍/mL) was similar to that of Trolox, which was noted as a major antioxidant in Yellowball peel. Further studies on the antioxidant capacity of Yellowball peel are required; however, these results provide a foundation for using Yellowball peel as an antioxidant.

• 한국식품과학회지
• /
• 제43권5호
• /
• pp.553-557
• /
• 2011

마늘의 천연 성분을 분석하였을 때 8개의 주요 성분이 나타났으며, 가장 크게 나타난 피크는 알린이었고 실제로 함량도 가장 높게 나타났다. 이소알린은 알린의 뒤를 이어 큰 피크를 나타내었고 함량도 알린에 이어 많은 양이 얻어졌다. 기타 마늘 특유의 함황유기화합물로서 ${\gamma}$-glutamyl peptide류가 있으며 함량이 충분하여 분리 정제를 수행한 것으로는 ${\gamma}$-glutamyl-S-allylcysteine, ${\gamma}$-glutamyl-S-1-propenylcysteine, ${\gamma}$-glutamylphenylalanine 등 3가지였다. 기타 마늘 특유의 성분은 아니지만 UV 208 nm에서 흡광도를 크게 나타내는 것으로 arginine, tyrosine, phenylalanine, tryptophan과 같은 일반적인 아미노산류가 있었지만, 본 연구에서는 마늘 특유의 아미노산과 펩타이드만을 정제하였다. 마늘 특이 아미노산과 펩타이드의 분리정제는 재순환 분취 HPLC를 이용하여 순수하게 정제하였으며, 생마늘 6 kg으로부터 알린, 이소알린, ${\gamma}$-glutamyl-S-allylcysteine, ${\gamma}$-glutamyl-S-1-propenylcysteine, ${\gamma}$-glutamylphenylalanine이 각각 7.32, 1.53, 0.38, 0.42, 0.23 g을 얻었으며 이를 마늘 함유량 대비 수율로 계산하면 각각 12.2, 42.5, 1.6, 1.2, 4.8%이었다. 정제한 물질들의 동정방법은 HPLC 머무름 시간의 비교 및 LC/MS를 이용한 분자량 측정이었다. 동일한 분자량을 가지는 알린과 이소알린을 분별하기 위해 $^1H$-NMR를 그리고 ${\gamma}$-glutamyl-S-allylcysteine과 ${\gamma}$-glutamyl-S-1-propenylcysteine을 구별하기 위해 $^1H$-NMR과 $^{13}C$-NMR분석을 수행하였다.

• 한국약용작물학회지
• /
• 제27권6호
• /
• pp.419-426
• /
• 2019

Background: This study aimed to identify antioxidant compounds from the seeds of Dolichos lablab L. by bioassay-guided isolation and recrystallization. Methods and Results: The water layer of D. lablab L. seed extract inhibits intracellular reactive oxygen species (ROS) expressing the 2',7'-dichlorofluorescein diacetate (DCF-DA), Cu/Zn superoxide dismutase (SOD) and catalase genes, as determined by quantitative real-time PCR (qRT-PCR). Two compounds were purified from the water layer of the seeds of D. lablab L. using column chromatography and prep-high performance liquid chromatography (HPLC). Using nuclear magnetic resonance (NMR) and electrospray Ionization mass spectrometry (ESI-MS), their chemical structures were identified as 5-[(2-acetyl-2,3-dihydro-1H-indazol-1-yl)carbonyl]-4,5-dihydro-3H-furan-2-one (C₁₄H₁₄N₂O₄) and stachyose. Conclusions: Two active antioxidant compounds were purified from the seed extract of D. lablab L. seed extract and the structures of these compounds were identified as C₁₄H₁₄O₄N₂ and stachyose.

• KSBB Journal
• /
• 제9권5호
• /
• pp.469-474
• /
• 1994

본 연구의 목적은 시판 퍼l녹시계 제초제 2,4-D의 생물학적 처리의 가능성을 평가하기 위한 것이다. 시판 페녹시계 제초제는 2,4-0 아민염 으로셔 2,4-0( 40%)와 용제 (60 % )로 구성 되었다. 2,4-D에서 농화배양에 의해 얻어진 미생물 컨소시염은 탄소원 빛 에너지원으로서 2,4-0를 이용하였다. 이 설험에서 2,4-D분해의 최적 pH 와 기 질농도는 각각 7.0과 54mg/ E 였다. Yeast extract와 ascorbic acid의 첨가는 2,4-0의 분해 와 미생물의 생장을 촉진시켰다. 2,4-0를 정량하기 위해 HPLC가 사용되었으며 그 과정에셔 중간대사물질로셔 2,4-0CP가 분리되었다. GC MS는 2,4-0CP를 입증하기 위하여 사용되였다. 배양중의 UV scans 결과, 2,4-0의 최대흡광치는 배양이 진행되는 동안 감소되었으나, spectral 및 peak 변화는 보여주지 않았다.

• 한국버섯학회지
• /
• 제20권4호
• /
• pp.187-192
• /
• 2022

Wolfiporia cocos is an edible fungus commercially cultivated in Asia. To investigate metabolic changes of W. cocos mycelia under both light and dark culture conditions, gas chromatography mass spectrometry (GC-MS) and high-performance liquid chromatography (HPLC) analyses were performed. In terms of the total amount of sugars, alcohols, amino acids, organic acids, fatty acids, and purines, there no significant differences between the W. cocos mycelia cultivated under light (L) or dark (D) conditions (p < 0.05). However, there were some differences with respect to the production of particular sugars and proteins. The levels of trehalose (L: 17.2 ± 0.3% vs. D: 13.9 ± 1.6%), maltose (L: 0.9 ± 0.1% vs. D: 0.3 ± 0.1%), turanose (L: 0.7 ± 0.2% vs. D: 0.1 ± 0.1%), glutamine (L: 1.6 ± 0.3% vs. D: 0.7 ± 0.2%), and proline (L: 0.3 ± 0% vs. D: 0.1 ± 0%) were all significantly higher under light condition (p < 0.05). In contrast, the levels of galactose (L: 13.7 ± 1.2% vs. D: 17.6 ± 2.0%), aspartic acid (L: 0.6 ± 0.1 % vs. D: 0.9 ± 0.1%), cystathionine (L: 0.6 ± 0.1% vs. D: 0.8 ± 0 %), and malic acid (L: 0.7 ± 0.1% vs. D: 1.2 ± 0.1%) were higher under the dark condition. It is worth noting that the amount of pachymic acid, a pharmaceutically active compound of W. cocos, was 1.68 times greater under the light condition (p < 0.05).

• Journal of Plant Biotechnology
• /
• 제47권1호
• /
• pp.78-89
• /
• 2020

기능성 성분이 향상된 토마토 품종 개발을 위해서는 성분 정량분석법과 토마토 유전자원 간 대사성분 변이에 대한 정보의 확보가 필요하다. 본 연구에서는 토마토 유전자원23개 계통과 12개 상용 F₁ 품종을 이용하여 수용성 비타민 7종(vitamin C, B1, B2, B3, B5, B6, B9)과 폴리페놀계 성분 5종(quercetin, rutin, kaempferol, myricetin, and naringenin chalcone)에 대한 함량을 비교 분석 하였다. HPLC와 LC-MS 분석 결과, 수용성 비타민과 폴리페놀계의 주요 성분으로 vitamin C와 naringenin chalcone이 각각 검출되었으며 품종 간 높은 수준의 함량 변이가 존재함을 알 수 있었다. 반면에 vitamin B1, quercetin 과 kaempferol은 전 품종에 있어 함량이 가장 낮았다. 대사성분 함량과 토마토 과실특성 간 상관관계에 있어 서 과크기(과중)와 높은 유의성이 관찰되었는데 대부분의 성분에 있어 방울토마토 품종이 완숙용 토마토 품종보다 높은 함량을 보였다. 하지만 naringenin chalcone을 제외하고 대사성분과 과색 간의 상관관계는 뚜렷하게 나타나지 않았다. 본 결과는 토마토 육종과정에 활용될 수 있는 효율적인 대사성분 정량분석법을 제시할 뿐만 아니라 기능성 성분 고함량 육종소재 선발에 중요한 정보를 제공한다.

• 한국토양비료학회지
• /
• 제45권1호
• /
• pp.43-50
• /
• 2012

Two typical animal waste management practices, composting and stockpiling, were evaluated for their effect on the degradation of three veterinary antibiotics (VAs), chlortetracycline (CTC), tylosin (TYL), and monensin (MNS). The VAs were applied to horse manure plots subject to composting or stockpiling, and core samples were collected over a period of time. Selected buffer solutions were used to extract the VAs and analysis for concentration was conducted with solid phase extraction (SPE) followed by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) technique. The VAs demonstrated rapid dissipation within ten days followed by a gradual decrease in concentration until the end of the experimental period (141 days). All three VAs degraded more rapidly in the composting samples than in the stockpiling samples, particularly between 20 and 60 days of the observation period. Degradation of the three VAs generally followed a first-order kinetic model, and a fitted model with a calculated rate constant was determined for each treatment. TYL in composting showed the fastest degradation, with a calculated rate constant of $0.91day^{-1}$; the slowest degradation was exhibited by MNS in stockpiling, with rate constant of $0.17day^{-1}$. Calculated correlation coefficients ranged from 0.89 to 0.96, indicating a strong correlation between measured concentrations and fitted values in this study. Although concentration of TYL in composting treatment showed below detection limit during the test period, this study suggests that composting can reduce animal waste contaminants prior to field application as fertilizer.

• 한국토양비료학회지
• /
• 제49권3호
• /
• pp.242-250
• /
• 2016

Veterinary antibiotics (VAs) has been used to treat animal disease and to increase animal weight as growth promoter. However, abused usage of VAs can cause production of antibiotic resistance genes (ARGs) in the environment and additionally, residual of VAs in soil can be transferred into crops. Therefore, main objective of this research was to examine bioaccumulation of VAs in sprouts (red cabbage, Brassica Olearacea L. var. Capitata f. rubra and red radish, Raphanus sativus) with hydroponic method. Total of 7 VAs in 2 different classes of VAs (tetracyclcines: tetracycline, oxytetracycline, chlortetracycline, sulfonamides: sulfamethoxazole, sulfamethazine, sulfamethiazole, macrolides: tylosin) were evaluated and experiment was conducted with solid phase extraction (SPE)/high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). Initial spiked concentration of 7 VAs was $5mg\;L^{-1}$ and cultivation period was 8 days. Result showed that growth of sprouts was inhibited about 23-27% when VAs was introduced. Amount of bioaccumulated VAs was also differed depending on class of VAs. The highest amount of bioaccmulated VAs was tetracycline and sulfamethoxazole in each class with a concentration of 4.05, $7.73mg\;kg^{-1}$ respectively. Calculated transfer ratio of VAs into crops was also ranged 0.38-54.27%. Overall, bioaccumulation of VAs in crops can be varied depending on crop species and class of VAs. However, further research should be conducted to verify bioaccumulation of VAs in crops in the soil environment.

• 약학회지
• /
• 제51권2호
• /
• pp.133-139
• /
• 2007

A simple and sensitive HPLC-MS method for quantitation of 10${\alpha}$-methoxy-9,10-dihydrolysergol (MDL), the main metabolite of nicergoline, in human plasma was developed and the bioavailability parameters of MDL was assessed in Korean healthy male volunteers. Clomipramine was used as an internal standard. MDL and internal standard in plasma sample were extracted using ethyl acetate. A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 10 mM ammonium acetate-acetonitrile (10 : 90, v/v). The reconstituted samples were injected into a Zorbax SB-C8 column (2.1${\times}$150 mm,5 ${\mu}$m) at a flow-rate of 0.3 ml/min. Using MS with selected ion monitoring (SIM) mode, MDL and clomipramine were detected without severe interference from human plasma matrix. MDL produced a protonated molecular ion ([M+H]$^+$) at m/z 287. Internal standard produced a protonated molecular ion ([M+H]$^+$) at m/z 315. A linear relationship for MDL was found in the range of 2.5${\sim}$100 ng/ml. The lower limit of quantitation (LLOQ) was 2.5 ng/ml with acceptable precision and accuracy. The intra- and inter-day validation for all coefficients of variation (R.S.D.%) were found less than 15%. Main pharmacokinetic parameters of 30 mg of nicergoline were revealed as follows: AUC$_t$ 321.1${\pm}$64.5 ng${\cdot}$hr/ml, C$_{max}$, 51.2${\pm}$25.3 ng/ml, T$_{max}$ 3.6${\pm}$1.5 hr, K$_{el}$ 0.12${\pm}$0.07 hr$^{-1}$ and t$_{1/2}$ 7.6${\pm}$3.4 hr. Inter subject variations and race differences were shown in comparison with the published data in the literature.