• Title/Summary/Keyword: tandem mass spectrometry coupled with liquid chromatography

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Evolution of 49 Phenolic Compounds in Shortly-aged Red Wines Made from Cabernet Gernischt (Vitis vinifera L. cv.)

  • Li, Zheng;Pan, Qiu-Hong;Jin, Zan-Min;He, Jian-Jun;Liang, Na-Na;Duan, Chang-Qing
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.1001-1012
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    • 2009
  • A total of 49 phenolic compounds were identified from the aged red wines made from Cabernet Gernischt (Vitis vinifera L. cv.) grapes, a Chinese characteristic variety, including 13 anthocyanins, 4 pryanocyanins, 4 flavan-3-ol monomers, 6 flavan-3-ol polymers, 7 flavonols, 6 hydroxybenzoic acids, 5 hydroxycinnamic acids, 3 stilbenes, and 1 polymeric pigment. Evolution of these compounds was investigated in wines aged 1 to 13 months. Variance analysis showed that the levels of most phenolics existed significant difference in between wines aged 3 and 9 months. Cluster analysis indicated that 2 groups could be distinguished, one corresponding to wines aged 1 to 3 months and the other to wines aged 4 to 13 months. It was thus suggested that there were 2 key-stages for the development of fine wine quality, at the aged 3 and 9 months, respectively. This work would provide some helpful information for quality control in wine production.

Analysis of Aminoglycoside Antibiotics in Meat and Cell Culture Medium Coupled with Direct Injection of an Ion-pairing Reagent (이온쌍 시약 직접 주입법을 활용한 육류 및 세포배양액 내 아미노글리코사이드계 항생제 분석)

  • Kyung-Ho Park;Song-Yi Gu;Geon-Woo Park;Jong-Jib Kim;Jong-soo Lee;Sang-Gu Kim;Sang-Yun Lee;Hyang Sook Chun
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.319-331
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    • 2023
  • Aminoglycoside antibiotics, also known as aminoglycosides (AGs), are veterinary drugs effective against a wide range of gram-negative and gram-positive bacteria. Owing to their recent use in cultured meats, it has become essential to establish an analytical method for safety management. AGs are highly polar compounds, and ion-pair reagents (IPRs) are used to ensure component separation. Owing to the high possibility of potential mechanical problems resulting from IPR addition to the mobile phase, an analytical method in which IPRs are added directly to the vial was explored. In this study, methods for analyzing 10 AGs via liquid chromatography-tandem mass spectrometry (LC-MS/MS) with the addition of two IPRs were validated for selectivity, detection limit, quantitation limit, recovery, and precision. The detection limit was 0.0001-0.0038 mg/kg, the quantification limit was 0.004-0.011 mg/kg, and the linearity (R2) within the concentration range of 0.01-0.5 mg/kg was over 0.99. Recovery and precision (expressed as relative standard deviation) evaluated in the two matrices (beef and cell culture media) ranged from 70.7% to 120.6% and 0.2% to 24.7%, respectively. The validated AG analytical method was then applied to 15 meats prepared from chicken, beef, and pork, and 6 culture media and additives used in cultured meat. No AGs were detected in any of the 15 meats distributed in Korea; however, streptomycin and dihydrostreptomycin were detected at levels ranging from 695.85 to 1152.71 mg/kg and 6.35 to 11.11 mg/kg, respectively, in the culture media additives. The LC-MS/MS method coupled with direct addition of IPRs to the vial can provide useful basic data for AG analysis and safety evaluation of meats as well as culture media and additives for cultured meats.

Chemical transformation and target preparation of saponins in stems and leaves of Panax notoginseng

  • Wang, Ru-Feng;Li, Juan;Hu, Hai-Jun;Li, Jia;Yang, Ying-Bo;Yang, Li;Wang, Zheng-Tao
    • Journal of Ginseng Research
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    • v.42 no.3
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    • pp.270-276
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    • 2018
  • Background: Notoginsenoside Ft1 is a promising potential candidate for cardiovascular and cancer disease therapy owing to its positive pharmacological activities. However, the yield of Ft1 is ultralow utilizing reported methods. Herein, an acid hydrolyzing strategy was implemented in the acquirement of rare notoginsenoside Ft1. Methods: Chemical profiles were identified by ultraperformance liquid chromatography coupled with quadruple-time-of-flight and electrospray ionization mass spectrometry (UPLC-Q/TOF-ESI-MS). The acid hydrolyzing dynamic changes of chemical compositions and the possible transformation pathways of saponins were monitored by ultrahigh-performance LC coupled with tandem MS (UHPLC-MS/ MS). Results and conclusion: Notoginsenoside Ft1 was epimerized from notoginsenoside ST4, which was generated through cleaving the carbohydrate side chains at C-20 of notoginsenosides Fa and Fc, and vinaginsenoside R7, and further converted to other compounds via hydroxylation at C-25 or hydrolysis of the carbohydrate side chains at C-3 under the acid conditions. High temperature contributed to the hydroxylation reaction at C-25 and 25% acetic acid concentration was conducive to the preparation of notoginsenoside Ft1. C-20 epimers of notoginsenoside Ft1 and ST4 were successfully separated utilizing solvent method of acetic acid solution. The theoretical preparation yield rate of notoginsenoside Ft1 was about 1.8%, which would be beneficial to further study on its bioactivities and clinical application.

Reduced Ceramides Are Associated with Acute Rejection in Liver Transplant Patients and Skin Graft and Hepatocyte Transplant Mice, Reducing Tolerogenic Dendritic Cells

  • Hyun Ju Yoo;Yeogyeong Yi;Yoorha Kang;Su Jung Kim;Young-In Yoon;Phuc Huu Tran;Taewook Kang;Min Kyung Kim;Jaeseok Han;Eunyoung Tak;Chul-Soo Ahn;Gi-Won Song;Gil-Chun Park;Sung-Gyu Lee;Jae-Joong Kim;Dong-Hwan Jung;Shin Hwang;Nayoung Kim
    • Molecules and Cells
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    • v.46 no.11
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    • pp.688-699
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    • 2023
  • We set up this study to understand the underlying mechanisms of reduced ceramides on immune cells in acute rejection (AR). The concentrations of ceramides and sphingomyelins were measured in the sera from hepatic transplant patients, skin graft mice and hepatocyte transplant mice by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Serum concentrations of C24 ceramide, C24:1 ceramide, C16:0 sphingomyelin, and C18:1 sphingomyelin were lower in liver transplantation (LT) recipients with than without AR. Comparisons with the results of LT patients with infection and cardiac transplant patients with cardiac allograft vasculopathy in humans and in mouse skin graft and hepatocyte transplant models suggested that the reduced C24 and C24:1 ceramides were specifically involved in AR. A ceramide synthase inhibitor, fumonisin B1 exacerbated allogeneic immune responses in vitro and in vivo, and reduced tolerogenic dendritic cells (tDCs), while increased P3-like plasmacytoid DCs (pDCs) in the draining lymph nodes from allogeneic skin graft mice. The results of mixed lymphocyte reactions with ceranib-2, an inhibitor of ceramidase, and C24 ceramide also support that increasing ceramide concentrations could benefit transplant recipients with AR. The results suggest increasing ceramides as novel therapeutic target for AR, where reduced ceramides were associated with the changes in DC subsets, in particular tDCs.

Gintonin facilitates brain delivery of donepezil, a therapeutic drug for Alzheimer disease, through lysophosphatidic acid 1/3 and vascular endothelial growth factor receptors

  • Choi, Sun-Hye;Lee, Na-Eun;Cho, Hee-Jung;Lee, Ra Mi;Rhim, Hyewhon;Kim, Hyoung-Chun;Han, Mun;Lee, Eun-Hee;Park, Juyoung;Kim, Jeong Nam;Kim, Byung Joo;Nah, Seung-Yeol
    • Journal of Ginseng Research
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    • v.45 no.2
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    • pp.264-272
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    • 2021
  • Background: Gintonin is a ginseng-derived exogenous G-protein-coupled lysophosphatidic acid (LPA) receptor ligand, which exhibits in vitro and in vivo functions against Alzheimer disease (AD) through lysophosphatidic acid 1/3 receptors. A recent study demonstrated that systemic treatment with gintonin enhances paracellular permeability of the blood-brain barrier (BBB) through the LPA1/3 receptor. However, little is known about whether gintonin can enhance brain delivery of donepezil (DPZ) (Aricept), which is a representative cognition-improving drug used in AD clinics. In the present study, we examined whether systemic administration of gintonin can stimulate brain delivery of DPZ. Methods: We administered gintonin and DPZ alone or coadministered gintonin with DPZ intravenously or orally to rats. Then we collected the cerebral spinal fluid (CSF) and serum and determined the DPZ concentration through liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Results: Intravenous, but not oral, coadministration of gintonin with DPZ increased the CSF concentration of DPZ in a concentration- and time-dependent manner. Gintonin-mediated enhancement of brain delivery of DPZ was blocked by Ki16425, a LPA1/3 receptor antagonist. Coadministration of vascular endothelial growth factor (VEGF) + gintonin with DPZ similarly increased CSF DPZ concentration. However, gintonin-mediated enhancement of brain delivery of DPZ was blocked by axitinip, a VEGF receptor antagonist. Mannitol, a BBB disrupting agent that increases the BBB permeability, enhanced gintonin-mediated enhancement of brain delivery of DPZ. Conclusions: We found that intravenous, but not oral, coadministration of gintonin facilitates brain delivery of DPZ from plasma via LPA1/3 and VEGF receptors. Gintonin is a potential candidate as a ginseng-derived novel agent for the brain delivery of DPZ for treatment of patients with AD.

Method Development for Determination of Trichothecene Mycotoxins in Nuts by LC-MS/MS (LC-MS/MS를 이용한 견과류 중 트리코테센계 곰팡이 독소 10종 동시분석법 개발)

  • Kim, Dan-Bi;Park, Ji-Su;Yoo, Mi-Young
    • Journal of Food Hygiene and Safety
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    • v.33 no.5
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    • pp.354-360
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    • 2018
  • This study presents a method validation for extraction and quantitative analysis of trichothecene mycotoxins in nuts based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach for extraction and enhanced matrix removal (EMR)-lipid-disperive-SPE (d-SPE) cleanup method, with detection and quantification by high-performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) in positive- and negative-ion modes. Linearity, precision, and accuracy were validated for LC-MS/MS methods. Results obtained with LC-MS/MS were linear, with correlation coefficient ($R^2$) of 0.998. Limits of detection and quantification for mycotoxins were $0.41-3.57{\mu}g/kg$ and $1.23-10.82{\mu}g/kg$, respectively. Intra- and inter-day precisions (RSD, %) were 0.40-8.44% and 1.93-12.46%, respectively. Results indicated to be rapidly and accurately identifying trichothecene mycotoxins and may be used as a suitable safety management method for nuts and nuts related commodities.

Residual characteristics of insecticide flubendiamide in kale (케일 중 살충제 Flubendiamide의 잔류 특성)

  • Kim, Hyun-Jin;Hwang, Kyu-Won;Sun, Jung-Hun;Lee, Tae-Hyun;Jeong, Kyoung-Su;Moon, Joon-Kwan
    • Journal of Applied Biological Chemistry
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    • v.65 no.3
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    • pp.173-181
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    • 2022
  • This study was carried out to investigate the residual characteristics of flubendiamide in kale to establish pre-harvest residue limits (PHRL) and the removal efficiency according to the washing solvent and method. Field tests were conducted at two different greenhouses, field 1 (Anseong-si, Gyeonggi-do) and field 2 (Incheon-si, Gyeonggi-do). According to the safe use guidelines kale was sprayed with flubendiamide twice every 10 days and harvested 0 (after 2 h), 1, 2, 3, 5, 7 and 10 days after the final application. The biological half-live of flubendiamide in kale was calculated based on dissipation curves of the pesticide in samples analyzed by liquid chromatography coupled with tandem mass spectrometry. In the analysis, method limits of quantitation (MLOQ) were 0.01 mg/kg, and recoveries performed with two different fortification levels of 10 MLOQ and maximum residue limit (0.7 mg/kg) were 104.2±3.6 and 101.9±10.2%, respectively. The dissipation rate constant of flubendiamide in kales were 0.2437 at field 1 and 0.1981 at field 2. PHRL calculation equations obtained using the dissipation constants estimated as follows: if the residual concentration of flubendiamide in kale on 10 days before harvest is less than 8.0 mg/kg, the residual concentration on the harvest would be under MRL. The removal of flubendiamide from kale was the greatest when it was washed with vinegar (39.8%), followed by baking soda (31.7%), calcium powder (30.2%), neutral detergent (27.2%), and tap water (15.9%). The results of this study would be useful for both farmers and consumers to produce or consume safe agricultural products.

Monitoring of illegal compounds and prohibited natural ingredients in foods (식품 중 발기부전치료제 및 사용금지 성분 모니터링)

  • Yun, Jisuk;Choi, Jangduck;Kwon, Kisung;Jo, Cheon-Ho
    • Korean Journal of Food Science and Technology
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    • v.48 no.5
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    • pp.405-412
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    • 2016
  • Illegally adulterated compounds, such as impotency drugs and their synthetic analogues, which have been purported to enhance sexual potency or mood, have been constantly detected in foods including dietary supplements. The adulterated foods with these illegal compounds may threaten public health because their safety and efficacy have not been verified. This study was aimed at investigating illegal compounds in foods and counterfeit products. 54 illegal compounds were assayed using a simultaneous analytical method involving liquid chromatography equipped with photo diode array (LC-PDA) and LC coupled with tandem mass spectrometry (LC-MS/MS). The method was validated in terms of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy. In 48 of 161 samples, we identified 7 different illegal compounds, including sildenafil, tadalafil, chlropretadalafil, demethylsildenafil, dimethyl-thiosildenafil, icariin and yohimbine. When purchasing products marketed for erectile dysfunction or aphrodisiacs, ulmost care should be taken owing to the possible presence of these illegal compounds.

Screening of anti-obesity drugs, their analogues and prohibited ingredients in slimming foods (식품 중 부정 혼입된 비만치료제 및 사용금지 성분 실태조사)

  • Yun, Jisuk;Choi, Jangduck;Kwon, Kisung;Jo, Cheon-Ho
    • Korean Journal of Food Science and Technology
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    • v.48 no.5
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    • pp.424-429
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    • 2016
  • Globally, obesity has been recognized as a serious health problem. Recently, slimming foods for weight loss and maintenance were found to contain anti-obesity drugs, their analogues, and prohibited ingredients. To avoid inspections by the Government, structurally modified analogs have been continuously synthesized. For rapid determination of adulterated slimming products, we simultaneously analyzed 21 illegal compounds using liquid chromatography (LC) equipped with photo diode array, and LC coupled with tandem mass spectrometry. The validation of the method was performed with regard to selectivity, linearity, limit of detection, limit of quantification, precision, and accuracy. We purchased 128 samples from the Korean market and online sources in the year 2015. In 31 samples, 3 illegal compounds were detected as follows: 9.9-135.3 mg/g of sibutramine, 0.2-17.5 mg/g of yohimbine, and 1.8 mg/g of icariin. This simultaneous detection method might prove to be a simple and rapid analysis for monitoring illegal compounds in slimming foods.

Determination of Phenolic Contents in Rooibos (Asphalthus linearis) Tea Depending on the Steeping Temperature and Time (루이보스차(Asphalthus linearis)의 추출방법에 따른 페놀릭류 함량 변화연구)

  • Park, Sin-Hee;Do, Yung-Suk;Kim, Youn-Sung;Kim, Nan-Young;Lee, Jin-Hee;Kim, Jong-Hwa;Yoon, Mi Hye
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.389-395
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    • 2017
  • A simultaneous determination of 5 phenolic acids (gallic acid, chlorogenic acid, caffeic acid, pcoumaric acid, trans ferulic acid) and 9 flavonoids (procyanidin b1, aspalathin, rutin, vitexin, hyperoside, isoquercitrin, luteolin, quercetin, chrysoeriol) in rooibos tea has been carried out by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). A validated analysis method in this study was applied to rooibos aqueous infusions. Rooibos tea is an antioxidant-rich tea which has anti-cancer, anti-aging, anti-inflammatory, anti-diabetic effect. Extraction yield of phenolics depends on steeping time and temperature of water. Tea infusions were prepared by placing 1 g of tea leaves or 1 tea bag in 100 mL of boiled water, and then at 3, 6 and 30 minutes intervals the infused teas were taken to carry out the analysis of phenolic contents. Another tea infusion was conducted with cold water ($25-30^{\circ}C$) for 30 minuntes. As a result, the total amount of phenolics was highest in rooibos tea steeped with hot water for 30 minutes, followed by 6 minutes, 3 minutes and cold water 30minutes and the result has statistical significance.