• Title/Summary/Keyword: HPLC-MS-MS

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Analysis of Free Amino Acids and Flavors in Fermented Jujube Wine by HPLC and GC/MS (GC-MS 및 HPLC를 이용한 대추발효주의 유리 아미노산 및 향기성분 분석)

  • Chun, Myoung Sook;Kim, Soon Jin;Noh, Bong Soo
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.779-784
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    • 2012
  • Characteristic chemical compositions of jujube wine using different preparation methods including fermentation were investigated. Fermentation for jujube wine started using whole fruit (JW1), seed-removed fruit (JW2) and whole fruit heated at $100^{\circ}C$ for 2 h and then extracted (JW3). The free amino acids and flavors were analyzed quantitatively by HPLC and GC-MS. A total of 18 amino acids were identified in all samples. The amount of total free amino acids was detected from 141-210 ppm (JW1), 147-342 ppm (JW2), and 336-362 ppm (JW3). Large amounts of proline, aspartate, glutamate, arginine and alanine were detected in jujube wine. Thirteen kinds of volatile compounds including six alcoholic compounds (ethyl alcohol, iso-butyl alcohol, n-butyl alcohol, iso-amyl alcohol, n-amyl alcohol, and phenethyl alcohol), four ester (ethyl acetate, hexyl acetate, ethyl caprylate, and phenethyl acetate) and three aldehydes (diethylacetal, furfural, and benzaldehyde) were detected. Ethyl alcohol (30.50-33.95% peak area), benzaldehyde (2.55-15.97% ratio), furfural (0.07-15.28% ratio), iso-amyl alcohol (1.04-14.73% ratio), and phenethyl acetal (0.78-9.28% ratio) were abundant in jujube wine.

Development Rapid Analytical Methods for Inositol as a Trace Component by HPLC and LC-MS/MS in Infant Formula

  • Shin, Jin-Ho;Park, Jung-Min;Kim, Ha-Jung;Ahn, Jang-Hyuk;Kwak, Byung-Man;Kim, Jin-Man
    • Food Science of Animal Resources
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    • v.35 no.4
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    • pp.466-472
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    • 2015
  • A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

Evaluation of Pre-treatment Stages for Microcystins Analysis using LC/MS/MS (LC/MS/MS 분석을 위한 microcystins 전처리 단계별 효율성 연구)

  • Kim, Hwa-Bin;Park, Hae-Kyung;Moon, Jeong-Suk
    • Journal of Korean Society on Water Environment
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    • v.25 no.5
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    • pp.720-726
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    • 2009
  • We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

Analysis of Phoxim Residue in Animal Food Production (Cattle and Pig) by LC/ESI-MS/MS (LC/ESI-MS/MS를 이용한 식육(소, 돼지)중 잔류 phoxim 분석)

  • Park, Mi-Sun;Lee, Jin-Joo;Myung, Seung-Woon
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.626-632
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    • 2011
  • Phoxim, which is one of veterinary drugs, is a well-known antiparasitic agent in wide use. In this paper, phoxim was extracted from cattle and pig tissue using solid-phase extraction (SPE) employing a silica cartridge with acetonitrile. Liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) for the analysis of phoxim from animal tissue was presented. Phoxim was detected on a $C_{18}$ column ($2.1{\times}100\;mm$, $3.5\;{\mu}m$) using a mobile phase of 0.1% formic acid in water and acetonitrile. A linear correlation observed in the calibration curves for cattle (0.0048~2.0 mg/kg) and pig (0.0055~2.0 mg/kg) showed above $r^2$=0.995. Accuracy measured at concentrations ranging from 0.0048 to 0.2 mg/kg was the range of 68.2~106.9%. Limit of detection (LOD) and limit of quantitation (LOQ) were the range of 0.0014~0.0017 mg/kg and 0.0048~0.0055 mg/kg, respectively. The precision (RSD%) was below 11.2%.

Analysis of streptomycin in honey by LC-MS/MS (LC-MS/MS를 이용한 벌꿀 중 스트렙토마이신 분석)

  • Shim, Young-Eun;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.424-431
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    • 2008
  • Streptomycin, which is one of aminoglycoside antibiotics, has been widely used in the rearing of food-producing animals to prevent and treat diseases in cattle, pigs and poultry. Although not licensed in South Korea, streptomycin has also been used for the treatment of bacterial honeybee disease, such as European foulbrood in Third World countries. A reliable and effective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of streptomycin in honey. A established method was optimized the clean-up and extraction procedure for the trace determination, good precision and accuracy. And the chromatographic and tandem mass spectrometric parameters were also optimized. The precision (RSD) and accuracy (bias) in the concentration range of 5.0~50.0 ug/kg were 5.5~14% and -10.0~8.0%, respectively. Limit of detection was 0.75 ug/kg and recovery of streptomycin spiked at level of 10 ug/kg in honey was 74%. The established and validated method was applied to determine streptomycin in honey which was on the market.

Separation of Glabridin from Licorice by RP-HPLC (RP-HPLC를 이용한 감초에서 Glabridin의 분리)

  • 정용안;이광진;권문주;노경호
    • KSBB Journal
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    • v.18 no.5
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    • pp.408-411
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    • 2003
  • By reversed-phase high-performance liquid chromatography, the extraction and separation of glabridin by from licoricce root was performed in this work. The column efficiencies and resolutions of glabridin were investigated with mobile phase composition on the reversed-phase chromatographic system. The glabridin collected from licorice root was identified by LC/MS. The mobile phase used to extract glabridin were composed of ethanol, methanol, acetone, and ethyl acetate. For one-hour ultrasonic extraction with solvent of ethyl acetate, the favorable content of glabridin was obtained as 1.26g/kg. The glabridin was well separated in the mobile phase composition of 50/50 vol. % (acetonitrile/water).

Isolation and Identification of an Unauthorized Sildenafil Analogue in a Commercial Functional Food (시판 기능성식품으로부터의 실데나필 유도체 부정첨가물질의 분리 및 구조규명)

  • Baek, Du-Jong
    • Journal of the Korean Chemical Society
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    • v.54 no.4
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    • pp.443-446
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    • 2010
  • HPLC analysis of a commercial herb drink marketed as a functional food revealed to contain an unauthorized substance similar to sildenafil, the active ingredient of the prescription drug Viagra$^{(R)}$ approved for the treatment of male erectile dysfunction. In order to identify the illegal additive, the herb drink was extracted with methylene chloride, and the extract was purified further using semipreparative HPLC. The chemical structure of the isolated substance was elucidated based on IR, LC/MS-ESI, and NMR spectroscopy, which showed the characteristics similar to sildenafil with minor modification. The only difference was the substitution of the methylpiperazine moiety of sildenafil to the hydroxyethylpiperazine group of the illegal additive.

Determination of Total Aflatoxins in Foods by Parallelism of ELISA and LC/MS/MS (ELISA-LC/MS/MS 병행에 의한 식품 중 aflatoxins 분석)

  • Kim, Kyeong-Yeol;Nam, Min-Ji;Nam, Bo-Ram;Ryu, Hee-Jung;Song, Jeong-Eon;Shim, Won-Bo;Lee, Soo-Hyung;Chung, Duck-Hwa
    • Journal of Environmental Health Sciences
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    • v.36 no.1
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    • pp.52-60
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    • 2010
  • High performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS) have been widely used to quantify aflatoxins in food, but these methods are expensive, time-consuming, unsuitable for analysis of the routine screening of large sample numbers and require derivatization and high level techniques to perform. The objective of this study is to detect aflatoxins in a large number of foods by a high efficient analytical system of combined enzyme linked immunosorbent assay (ELISA) for screening and LC/MS/MS for confirmation. The samples spiked individually with aflatoxin $B_1$ (0.5 and 1.0 ng/g) and total aflatoxins (10 ng/g) were analyzed by ELISA and LC/MS/ MS, and the recoveries for ELISA and LC/MS/MS were 71.8~119.2% and 70.8~135.3%, respectively. A total of 378 samples (grains, nuts, soybean and fermented soybean foods, pepper and fermented pepper foods) were purchased from the six major cities in Korea and analyzed by ELISA-LC/MS/MS system. Twenty two (5.8%; peanut: 11, pistachio: 2, walnut: 6, almond: 1, pepper powder: 1, pepper paste: 1) out of 378 samples were screened as aflatoxin B1 positive by ELISA, but, 4 (1.1%; peanut: 2, pistachio:1, pepper powder: 1) out of the 22 samples screened were confirmed as aflatoxins positive at levels of 1.02~52.79 ng/g by LC/MS/MS. ELISA-LC/MS/MS system provides a more rapid, accurate and cost-effective method for the detection of aflatoxins in large number of samples.

Separation and identification of selenoproteins in selenium-enriched yeast (셀레늄이 강화된 이스트에서 셀레늄 단백질의 분리 및 확인)

  • Kim, Kyong-Mi;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.6
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    • pp.357-363
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    • 2013
  • Selenium-containing proteins were separated from selenium-enriched yeast (SEY) using Trizol$^{(R)}$ reagent followed by anion exchange (AE) chromatography. This method is simpler and less time consuming than electrophoresis. Five selenium containing proteins were identified by on-line AE HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry). Each protein was enzymatically hydrolyzed to seleno-amino acids and separated with RP (reverse phase) HPLC for the identification of selenoproteins.

Use of Lycopene, an Antioxidant Carotinoid, in Laying Hens for Egg Yolk Pigmentation

  • Kang, D.-K.;Kim, S.-I.;Cho, C.-H.;Yim, Y.-H.;Kim, H.-S.
    • Asian-Australasian Journal of Animal Sciences
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    • v.16 no.12
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    • pp.1799-1803
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    • 2003
  • The possibility of lycopene affecting egg yolk pigmentation was studied with lycopene diets containing 0, 4, 8, and $12{\mu}g/g$ meal, respectively. The addition of lycopene above $4{\mu}g/g$ meal significantly improved yolk color after four days of supplementation. The transfer of lycopene into egg yolk was confirmed by thin layer chromatography, and high-performance liquid chromatography-mass spectrometry (HPLC-MS). The deposition rate of lycopene into egg yolk was approximately 2%, which was quantitatively determined using a HPLC with a UV detector. The result indicates that lycopene is a good candidate for egg yolk pigmentation and for making functional eggs.