• Title/Summary/Keyword: HPLC/FLD

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Determination of Amino Acids on Wintertime PM2.5 using HPLC-FLD (HPLC-FLD를 이용한 겨울철 PM2.5 중 아미노산 성분 분석)

  • Park, Da-Jeong;Cho, In-Hwan;Bae, Min-Suk
    • Journal of Korean Society for Atmospheric Environment
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    • v.31 no.5
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    • pp.482-492
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    • 2015
  • Ground-based measurements were conducted from January 6 to 12 of 2015 for understanding characteristics of nitrogen containing carbonaceous aerosols as 16 amino acids at the Mokpo National University, Korea. The detailed amino acid components such as Cystine ($(SCH_2CH(NH_2)CO_2H)_2$) and Methionine ($C_5H_{11}NO_2S$) and their sources were analyzed by High-Performance Liquid Chromatography with Fluorescence Detection (HPLC-FLD) for behavior of secondary products in particulate matter. In addition, organic carbon (OC) and elemental carbon (EC) based on the carbonaceous thermal distribution (CTD), which provides detailed carbon signature characteristics relative to analytical temperature, and water soluble organic carbon (WSOC) by total organic carbon (TOC) analyzer were used to understand the carbon compound behaviors. The backward trajectories were discussed for originations of carbonaceous aerosols as well. Different airmasses were classified with the amino acids and OC thermal signatures. The results can provide to understand the aging process influenced by the long-range transport from East Sea area.

Analysis of Residual Fluoroquinolones Contents in Fish (어류 중 Fluoroquinolone계 항균제의 분석 및 잔류량 조사)

  • Park, Young-Ae;Yuk, Dong-Hyun;Kim, Su-Un;Kim, Jin-Ah;Park, Ae-Sook;Kim, Youn-Cheon;Kim, Moo-Sang
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.293-299
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    • 2012
  • The residual contents of fluoroquinolones in fish and shrimp were analyzed by using HPLC-FLD and LC-MS. The limit of detection (LOD) and limit of quantification (LOQ) for fluoroquinolones by HPLC-FLD were 0.0030-0.0083 and 0.0090-0.0252 mg/kg, respectively. Those by LC-MS were 0.0019-0.0040 and 0.0059-0.0122 mg/kg, respectively. Recoveries regarding ofloxacin, norfloxacin, pefloxacin, ciprofloxacin and enrofloxacin ranged from 76.4-104.6%. The detection rate of fluoroquinolones was 7.5% from a total of 268 samples. In only one Korean bullhead sample, the sum of ciprofloxacin and enrofloxacin contents was detected at a higher level than its maximum residue limits (MRL) of 0.1 mg/kg. Ofloxacin, norfloxacin and pefloxacin were not detected in any samples and detection rates of ciprofloxacin and enrofloxacin were 3.4% and 6.7%, respectively. In detection rate by species eel (2.6%), loach (2.2%), Korean bullhead (1.5%), carp (0.7%) and snakehead (0.4%) were in order.

Establishment of Analytical Method for Residues of Ethychlozate, a Plant Growth Regulator, in Brown Rice, Mandarin, Pepper, Potato, and Soybean Using HPLC/FLD

  • Kim, Jae-Young;Lee, Jin Hwan;Lee, Sang-Mok;Chae, Young-Sik;Rhee, Gyu-Seek;Chang, Moon-Ik
    • Korean Journal of Environmental Agriculture
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    • v.34 no.2
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    • pp.111-119
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    • 2015
  • BACKGROUND: Ethychlozate (ECZ) is a plant growth regulator of synthetic auxin for agricultural commodities (ACs). Accurate and sensitive method to determine ECZ in diverse ACs on global official purpose is required to legal residue regulation. As the current official method is confined to the limited type of crops with poor validation, this study was conducted to improve and extend the ECZ method using high-performance liquid chromatography (HPLC) in all the registered crops with method verification. METHODS AND RESULTS: ECZ and its acidic metabolite (ECZA) were both extracted from acidified samples with acetone and briefly purified by dichloromethane partition. ECZ was hydrolyzed to form ECZA and the combined ECZA was finally purified by ion-associated partition including hexane-washing. The instrumental quantitation was performed using HPLC/ FLD under ion-suppression of ECZA with no interference by sample co-extractives. The average recoveries of intra- and inter-day experiment ranged from 82.0 to 105.2% and 81.7 to 102.8%, respectively. The repeatability and reproducibility for intra- and inter-day measurements expressed as a relative standard deviation was less than 8.7% and 7.4%, respectively. CONCLUSION: Established analytical method for ECZ residue in ACs was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

Pretreatment of Fish for the determination of polycyclic aromatic hydrocarbons using alkali digestion (알칼리분해를 이용한 어류 중 다환방향족탄화수소의 전처리방법)

  • Hu, Soojung;Lee, Hyomin;Chae, Youngzoo;Yoo, Eun-Ah
    • Analytical Science and Technology
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    • v.18 no.5
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    • pp.403-409
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    • 2005
  • Polycyclic Aromatic Hydrocarbons(PAHs) contamination arises from several sources including processing of food(smoking, direct drying, cooking) and environmental contamination of air, water, or soil, the later being considered as the most important. In this study, to establish the analytical method for some PAHs[benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene, indeno(1,2,3-c,d)pyrene] in fish, alkali digestion time, extraction solvents, elution volume of florisil cartridge for clean-up have been optimized. The methodology involved saponification and extraction with n-hexane, clean-up on Sep-Pak florisil cartridges and determination by HPLC/FLD(High Performance Liquid Chromatography/Fluorescence Detector). Overall method recoveries for 8 PAHs spiked into these products ranged from 90 to 106%.

Analysis of Benzo(a)pyrene in Red Ginseng Beverage (홍삼음료 증 벤조피렌 분석)

  • Hu, Soo-Jung;Jin, Sun-Hee;Choi, Dong-Mi
    • Journal of Food Hygiene and Safety
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    • v.23 no.1
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    • pp.26-30
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    • 2008
  • Polycyclic Aromatic Hydrocarbons(PAHs) contamination arises from several source including processing of food(smoking, direct drying, cooking) and environmental contamination of air, water or soil. A red ginseng is produced by steaming the root followed by drying. The methodology involved extraction with n-hexane and washing with water, clean-up on Sep-Pak Florisil Cartridges and determination by HPLC/FLD. The mobile phase was a mixture of acetonitrile and water in 8:2 by the isocratic elution and the excitation wavelength of fluorescence detector was 294 nm and its emission wavelength was 404 nm. The average recovery was about 105% and the relative standard deviation was 0.5. The levels of benzopyrene in the selected red ginseng beverage samples were not detected.

The Residues of Enrofloxacin in Cultured Paralichthys olivaceus (양식산 넙치에서 Enrofloxacin의 잔류)

  • Seo, Jung Soo;Jeon, Eun Ji;Lee, Eun Hye;Jung, Sung Hee;Park, Myoung Ae;Jee, Bo Young;Kim, Na Young
    • Journal of fish pathology
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    • v.26 no.1
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    • pp.45-50
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    • 2013
  • Enrofloxacin is one of the normally used flouroquinolones in mammalian and fish but its withdrawal time and studies were remain obscure. The residual contents of enrofloxacin in fish muscle were analyzed by using HPLC-FLD. More than 0.1 mg/kg of ENR was detected in muscle tissues and the residues were found over 1 year after treatment. The concentration of ENR in Paralichthys olivaceus was not affected by water temperature and lasted for an extended amount of time. The spike recoveries of ENR in the muscle tissue ranged from 78% to 85%. From this results, we need the prescription by veterinarian or aquatic organism disease inspector in ENR usage to assure safety of fish. Future research is required to determine the recommendation dose of ENR for side effects and safety.

Applied Analysis for Metabolic Profiling of Trace-level Amino Acid in Biological Fluid (생체시료 중 미량 아미노산 대사 프로필을 위한 분석법 응용)

  • Nam, Hyung Wook;Park, Song-Ja;Pyo, Hee Soo;Paeng, Ki Jung
    • Analytical Science and Technology
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    • v.16 no.5
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    • pp.349-357
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    • 2003
  • The universality of low molecular weight metabolites (i.e. amino acids, steroid hormones) allows rapid and straightforward investigation of biochemistry of genetically un-characterized species. Thus in vivo metabolic profiling of amino acid in combination with multivariate data analysis (metabolomics) offers great potential in comparative biology. In this paper, amino acid profiles in biological fluid (media) were studied by using HPLC/FLD. HPLC procedure for amino acids require the formation of derivatives due to the low absorption of the free compounds. o-Phthalaldehyde (OPA) used in association with a thiol, such as 3-mercaptopropionic acid (3-MPA), is one of the most popular and sensitive reagents, which yield quickly fluorescent iso-indoles at room temperature. To improve unstability of OPA/3-MPA derivatization, we optimized injector programs for fixed injection times. Linear regressions for the standard curves were linear in the range 0.5 - 100.0 ppb, giving correlation coefficents above 0.99. The detection limit were 1.70 pmol(GLU) - 23.81 pmol(SER). It is practically useful when the amount of sample is very low on single cells.

Quantitative Analysis of Vitamin B5 and B6 Using High Performance Liquid Chromatography (고속액체크로마토그래피를 이용한 비타민 B5 및 B6의 정량 분석)

  • Kim, Gi-Ppeum;Hwang, Young-Sun;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.10
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    • pp.1186-1194
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    • 2017
  • Recently, many people have demanded reliable nutritional data even for minor-components. On the other hand, an analytical method for the analyses of vitamin $B_5$ and $B_6$ is lacking. Therefore, this study attempted to validate with accuracy and precision the analysis of vitamin $B_5$ and $B_6$ using a high-performance liquid chromatography (HPLC) method. The vitamin $B_5$ and $B_6$ contents were analyzed using an Agilent 1260 series HPLC system. YMC-Pack ODS-AM ($250{\times}4.6mm$ I.D.) and YMC-Pack Pro RS $C_{18}$ ($250{\times}4.6mm$ I.D.) columns were used for the analyses of vitamin $B_5$ and $B_6$, respectively. In the case of vitamin $B_5$, the flow rate was set to 1.0 mL/min by isocratic elution using the 50 mM $KH_2PO_4$ solution (pH 3.5)/acetonitrile (ACN) (95:5, v/v) with monitoring at 200 nm using HPLC/DAD, whereas the flow rate for vitamin $B_6$ was set to 1.0 mL/min of flow rate by isocratic elution using a 20 mM $CH_3CO_2Na$ solution (pH 3.6)/ACN (97:3, v/v) with monitoring by excitation at 290 nm and emission at 396 nm using HPLC/FLD. The column temperature was set to $30^{\circ}C$. The injection volume was $20{\mu}L$ for each experiment. The specificity of the accuracy and precision for vitamin $B_5$ and $B_6$ were also validated by HPLC. The results showed high linearity in the calibration curve for vitamin $B_5$ ($R^2=0.9998^{{\ast}{\ast}}$), the limit of detection (LOD) and limit of quantitation (LOQ) were 0.4 mg/L and 1.3 mg/L, respectively, In contrast, for the calibration curve of vitamin $B_6$, which showed high linearity ($R^2=0.9999^{{\ast}{\ast}}$), the LOD and LOQ were 0.006 mg/L and 0.02 mg/L, respectively.

A Survey of the Presence of Aflatoxins in Food (식품 중 아플라톡신 오염도 조사)

  • Park, Min-Jung;Yoon, Mi-Hye;Hong, Hae-Geun;Joe, Tae-Suk;Lee, In-Sook;Park, Jeong-Hwa;Ko, Hoan-Uk
    • Journal of Food Hygiene and Safety
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    • v.23 no.2
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    • pp.108-112
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    • 2008
  • A survey of total aflatoxin levels was conducted on 158 samples (nuts, fermented foods and their processed products) collected in local markets in Gyeonggi-do and Domestic Internet Site. The total aflatoxins were quantified by the immunoaffinity column clean-up method followed by high performance liquid chromatography (HPLC)-fluorescence detector (FLD). Aflatoxins were found in 45(28.5%) samples including 34 nuts and nut products, 7 soybean pastes, 1 meju, 1 bean product and 2 corn snacks with a range of $0.02{\sim}3.96\;{\mu}g/kg$. These results show that the contamination level of aflatoxin in foods consumed in Korea is low compared with the standard in Korea Food Code($10\;{\mu}g/kg$ as aflatoxin $B_1$). Aflatoxin $B_1$ content was increased in peanuts and com snacks during storage but it was decreased in doenjang (soybean paste).

Analysis of Zearalenone Contamination in Cereal-Based Products Using High Performance Liquid Chromatography-Fluorescence Detector and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (곡류가공품 중 제랄레논 오염도 조사)

  • Jang, Mi-Ran;Lee, Chang-Hee;Choi, In-Sun;Shin, Choon-Shik;Kim, Jin-Hee;Jang, Young-Mi;Kim, Dong-Sul;Ahn, Dong-Hyun
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.224-229
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    • 2011
  • Zearalenone (ZEA) is an estrogenic mycotoxin mainly produced by Fusarium graminerum, a species which colonizes a wide variety of cereals, including wheat, barley and processed products. A survey of ZEA contamination was conducted on 141 dried confectioneries, 59 breads and rice cakes, 135 noodles and 101 other products, for a total of 432 commercial samples. Samples were analyzed by high performance liquid chromatography with fluorescence detection (HPLC-FLD) after immunoaffinity clean-up and was confirmed by liquid chromatography tandem mass spectrometry (LCMS/MS). The limits of detection and quantification were 2.0 and $6.0{\mu}g/kg$, respectively. The recovery ranged from 80.2% to 98.4% in the cereal based product. ZEA was detected in 38 samples (8.8% incidence), including 3 snack, 2 biscuit and 33 other cereal products. The ZEA contamination levels were in the range of $5.38-53.76{\mu}g/kg$. Finally, LC-MS/MS analysis of the contaminated samples was conducted to confirm the detected ZEA, and all 38 samples showing ZEA by HPLC-FLD were confirmed by LC-MS/MS.