• Title/Summary/Keyword: High performance liquid chromatography-UV

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Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant (식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가)

  • Suh, Hee-Jae;Kim, Kyung-Su;Hong, Mi-Na;Lee, Chan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.3
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    • pp.342-351
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    • 2016
  • This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

Studies on the Determination Method of Natural Sweeteners in Foods - Licorice Extract and Erythritol (식품 중 감초추출물 및 에리스리톨 분석법에 관한 연구)

  • Hong Ki-Hyoung;Lee Tal-Soo;Jang Yaung-Mi;Park Sung-Kwan;Park Sung-Kug;Kwon Yong-Kwan;Jang Sun-Yaung;Han Ynun-Jeong;Won Hye-Jin;Hwang Hye-Shin;Kim Byung-Sub;Kim Eun-Jung;Kim Myung-Chul
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.258-266
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    • 2005
  • Licorice Extract and Erythritol, food additives used in korea, are widely used in foods as sweetener. Its application for use in food is regulated by the standard and specification for food additives but official analytical method far determination of these sweetener in food has not been established. Accordingly, we has been carried out to set up analytical method of the glycyrrhizic acid in several foods by the way of thin layer chromatography and high performance liquid chromatography glycyrrhizic acid is qualitative anaylsis technique consists of clean-up with a sep-pak $C_{18}$ cartridge, separation of the sweeteners by Silica gel 60 F254 TLC plate using 1-butanol:4Nammonia solution:ethanol (50:20:10) as mobile solvent. Also, the quantitative analysis for glycyrrhizic acid, was performed using Capcell prk $C_{18}$ column at wavelength 254nm and DW:Acetonitrile (62:38 (pH2.5)) as mobile phase. and we has been carried out to set up analytical method of the erythritol in several foods by the way of high performance liquid chromatography. erythritol is qualitative anaylsis technique consists of clean-up with a DW and hexane. The quantitative analysis for erythritol, was performed using Asahipak NH2P-50 column, Rl and DW:Acetonitrile (25:75) as mobile phase. The glycyrrhizic acid results determined as glycyrrhizic acid in 105 items were as follows; N.D$\∼$48.7ppm for 18 items in soy sauce, N.D$\∼$5.3ppm for 12 items in sauce, N.D$\∼$988.93ppm for 15 items in health food, N.D$\∼$180.7ppm for 26 items in beverages, N.D$\∼$2.6ppm for 8 items in alcoholic beverages repectively and ND for 63 items in the ethers. The erythritol results determined as erythritol in 52 items were as follows; N.D$\∼$155.6ppm for 13 items in gm, N.D$\∼$398.1ppm for 12 items in health foods repectively and ND for 45 items in the others.

Quantitatation of Benzoic and Sorbic Acids in Some Processed Foods of Korea (일부 한국 가공식품의 벤조산과 소르빈산의 함량 조사)

  • Mitra, Sanika;Han, Jang-Il;Lee, Ki-Teak;Kim, Seong-Ai
    • Food Science and Preservation
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    • v.16 no.6
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    • pp.789-796
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    • 2009
  • Benzoic acid (BA) and sorbic acid (SA) are the preservatives most commonly used in food. Although BA and SA are generally safe, some previous studies have shown that consumption of excessive amounts of these food additives can be a health hazard. The aim of this study was to determine the amounts of BA and SA in processed foods in Korea. Different brands of fruit juice, yogurt, cheese, dried fruits, jam, and margarine were purchased at a local market in Daejeon, Korea. Samples were analyzed by high-performance liquid chromatography (HPLC) using a UV detector. Chromatographic separation was achieved with a C18 column. Methanol acetate buffer (pH 4.4) at a 35:65 v/v ratio was used as the initial mobile phase to elute BA and SA. The detector wavelength was set at 254 nm. The average test results observed for BA concentrations in fruit juice, yogurt, cheese, dried fruits, jam, and margarine were $40.26{\pm}0.02$, $2.07{\pm}0.06$, $0.02{\pm}0.09$, $0.36{\pm}08$, $265.30{\pm}0.02$, and $27.34{\pm}0.08\;mg/kg$, respectively. Average concentrations of SA in these samples were $0.92{\pm}0.06$, $1.06{\pm}0.07$, $7.30{\pm}0.01$, $14.14{\pm}0.08$, $25.65{\pm}0.06$, and $4.81{\pm}0.07\;mg/kg$, respectively. Thus, the average levels of BA and SA in the studied food items were lower than the KFDA-permitted limits. Moreover, the estimated daily intake of both BA and SA by a typical consumer were below the maximum recommended daily values.

A Study on Qualitative and Quantitative Analysis of Major ingredients in Scutellariae radix (황금(Scutellariae radix)의 주요 성분의 정성 및 정량분석에 관한 연구)

  • Rhee, Jae-Seong;Woo, Eun Ran;Kim, Nam-Hyuk;Lee, Eun-Ju;An, Duk-Kyun;Lee, Je-Hyun;Park, Seong Kyu;Park, Ho-Koon
    • Analytical Science and Technology
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    • v.10 no.2
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    • pp.91-104
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    • 1997
  • Scutellariae radix has been used on the control of body fever as oriental medicine for thousand years. Analytical aspect for the main components of Scutellariae radix was set up improving sensitivity and resolution. The analysis of 3 different flavonoids present in Scutellariae radix-baicalin, baicalein, wogonin-was conducted by means of high performance liquid chromatography with ODS reverse phase column in conjunction with a Photo Diode Array UV detector(280nm) at $40^{\circ}C$. Mobile phase was carried out at 1mL/min, composed of acetonitrile and 0.1M phosphoric acid in the form of a gradient method. Under these circumstances the retention time for baicalin, baicalein, wogonin was 7.65, 11.65 and 14.12 minutes respectively. As a result for the efficiency on extraction of active ingredients with proposed analytical process according to it's growing districts, Sunchang in Junbuk for baicalin and Bulkyo in, Junnam for bicalein and wogonin have shown the best results. Even the extraction at room temperature was satisfactory. Among acids, 0.1M acetic acid revealed the best achievements. The mixture of acetonitrile and 0.2M phosphoric acid(75:25) has been shown the best efficiency as well as stability for the extraction of active ingredients.

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Real-time monitoring for blending uniformity of trimebutine CR tablets using near-infrared and Raman spectroscopy (근적외분광분석법과 라만분광분석법을 이용한 트리메부틴말레인산 서방정의 혼합 과정 모니터링)

  • Woo, Young-Ah
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.519-526
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    • 2011
  • Chemometrics using near-infrared (NIR) and Raman spectroscopy have found significant uses in a variety quantitative and qualitative analyses of pharmaceutical products in complex matrixes. Most of the pharmaceutical can be measured directly with little or no sample preparation using these spectroscopic methods. During pharmaceutical manufacturing process, analytical techniques with no or less sample preparation are very critical to confirm the quality. This study showed NIR and Raman spectroscopy with principal component analysis (PCA) was very effective for the blending processing control. It is of utmost importance to evaluate critical parameters related to quality of products during pharmaceutical processing. The blending is confirmed by off-line determination of active pharmaceutical ingredient (API) by a conventional method such as high performance liquid chromatography (HPLC) and UV spectroscopy. These analytical methods are time-consuming and ineffective for real time control. This study showed the possibility for the determination of blend uniformity end-point of CR tablets with the use of both NIR and Raman spectroscopy. The samples were acquired from six positions during blending processing with U-type blender from 0 to 30 min. Using both collected NIR and Raman spectral data, principal component analysis (PCA) was used to follow the uniformity of blending and finally determine the end-point. The variation of homogeneity of six samples during blending was clearly found and blend uniformity end-point was successfully confirmed in the domains of principal component (PC) scores.

Determination of Vitamin B12 and Biotin in Foods for Special Dietary Uses with Immunoaffinity Column (면역친화성 컬럼을 이용한 특수용도식품 중 비타민B12와 비오틴 분석 연구)

  • Oh, Bo-Young;Ye, Min-Ji;Hu, Soo-Jung;Lee, Hye-Young;Bang, Soo-Jin
    • Journal of Food Hygiene and Safety
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    • v.35 no.3
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    • pp.252-260
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    • 2020
  • This study was conducted to improve the standard method for vitamin B12 and biotin contained in foods for special dietary uses to ensure the specificity of the complex matrix properties of foods. For the food code, the test method was improved to determine vitamin B12 and biotin by high-performance liquid chromatography (HPLC)-UV using column-switching after concentration using immunoaffinity column. The immunoaffinity columns contain a gel suspension of monoclonal antibody specific to the vitamin of interest so that it can be used to concentrate the vitamin B12 and biotin and remove interferences from the food extracts. Moreover, validation of advanced new methods was carried out to support the suitability of the proposed analytical procedure (specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision). The improved analytical method is being used to monitor relevant food items on sale. The results of this study showed that the new analytical method is suitable and appropriate for managing food intended for special dietary uses.

Pharmacokinetic analysis for the development of new potent anti-HIV-1 agents, the KR-V series (새로운 항HIV-1제, KR-V series의 개발을 위한 약물동태연구)

  • Lee, Young-mi;Kim, Jin-suk;Han, Sang-seop;Shin, Ho-chul
    • Korean Journal of Veterinary Research
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    • v.40 no.3
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    • pp.471-478
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    • 2000
  • The pharmacokinetic properties of KR-V compounds, recently developed as new anti-HIV agents, were studied after i.v. and p.o. administration in rats. The concentrations of the KR-V series were determined in rat plasma using an high-performance liquid chromatography (HPLC)-UV detection system. Of the 19 KR-V compounds investigated in the present study, only KR-V 3, 10, 14, 16 and 18-1 showed oral bioavailability. The plasma concentration-time data could be adequately described by an one-compartment open model. In the i.v. kinetic study (10mg/kg), the CLt of KR-V 3, 10, 14 and 16 (>4L/hr/kg) were significantly higher than that of KR-V 18-1 (1.1 L/hr/kg). The AUC of KR-V 18-1 was greater ($8.97{\mu}g{\cdot}hr/ml$) than that of the other compounds, but the Vd (0.58 L/kg) was lower. In the p.o. kinetic study (50mg/kg), although the t-1/2 of KR-V 18-1 was shorter than that of the other compounds, the AUC ($3.659{\mu}g{\cdot}hr/ml)$ and $C_{max}(1.891{\mu}g/ml$) were markedly higher. In a seperated in vitro experiment, only KR-V 18-1, of the 5 compounds with bioavailibility, exhibits potent activity against HIV-1 mutant strains. Therefore, KR-V 18-1 is expected to become a new potent anti-AIDS drug candidate/lead compound.

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Co-occurrence of Deoxynivalenol and Zearalenone in Cereals and their Products (곡류와 그 가공품에서 Deoxynivalenol과 Zearalenone의 분석)

  • Ok, Hyun-Ee;Chang, Hyun-Joo;Choi, Sung-Wook;Lee, Na-Ri;Kim, Hyun-Jung;Koo, Min-Sun;Chun, Hyang-Sook
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.375-381
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    • 2007
  • Deoxynivalenol (DON) and zearalenone (ZEN) are naturally occurring toxins produced by Fusarium species, which may grow on cereals. The aims of this study were to determine the incidence and contamination levels of DON and ZEN in cereal products. Seventy samples of cereal products were randomly selected from retail outlets during 2005 and 2006. DON and ZEN were analyzed by using high performance liquid chromatography with fluorescence and UV-detector, respectively. Detection limits were $4.4{\mu}g\;kg^{-1}$ for DON and $3.4{\mu}g\;kg^{-1}$ for ZEN. DON and ZEN were detected in 37 and 17, respectively, of the 70 samples, but the levels found were very low. In particular, out of 70 samples, 12 samples of corn and barley were co-contaminated with DON and ZEN, with levels ranging from 5.6 to $1842.3{\mu}g\;kg^{-1}$ for DON and 12.1 to $174.9{\mu}g\;kg^{-1}$ for ZEN, respectively. However, DON and ZEN were not detected in breakfast cereals and wheat flour. The highest level was found in dried corn kernel samples that confirmed by LC-MS. This study show that DON and ZEN co-contaminate with low levels in cereal products.

Residues of Thiamphenicol in Blood of Cultured Olive Flounder and Black Rockfish Treated by Single Oral Administration (Thiamphenicol의 단일 경구투여에 따른 넙치와 조피볼락의 혈액내 잔류 분석)

  • JUNG, Sung-Hee;SEO, Jung-Soo
    • Journal of Fisheries and Marine Sciences Education
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    • v.28 no.3
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    • pp.692-700
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    • 2016
  • This study was aimed at investigating the residual patterns of thiamphenicol (TP) in the cultured olive flounder (Paralichthys olivaceus) and black rockfish (Sebastes schlegeli) following oral administration. TP concentration were detected by high performance liquid chromatography with UV detector. The recovery rates of TP in serums ranged 77.05~97.23% (olive flounder) and 89.96~97.11% (black rockfish) for the concentration of 0.1, 1.0, $10{\mu}g/mL$, respectively. After single administration of TP (100 mg/kg body weight) by oral route in olive flounder ($700{\pm}50g$, $23{\pm}1.5^{\circ}C$) and black rockfish ($500{\pm}30g$, $23{\pm}1.5^{\circ}C$), the concentration in the serum was determined at 1, 5, 10, 15, 24, 30, 50, 168, 264 and 432 h post-dose. Two-compartment model was applied to analyze in the pharmacokinetics of TP administered to the fishes. In the serum of olive flounder, TP was detected on 10 and 15 hours after treatment were $10.08{\mu}g/mL$ and $10.06{\mu}g/mL$ as maximum level, respectively. In the serum of black rockfish, TP was detected on 15 hours after treatment were $8.88{\mu}g/mL$ as maximum level. Concentrations of TP to the fishes were not measurable at 432 hours (18 days) after treatment in all samples. Similar residual patterns of TP were revealed between the fishes. These results are helpful for estimating withdrawal time of TP which has been already in use for farmed fish treatment.

Development of Analytical Method for Rutin in Buckwheat Plant using High Performance Liquid Chromatography (메밀 식물체 함유 Rutin의 HPLC 분석방법 개발)

  • Choung Myoung-Gun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.50 no.spc1
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    • pp.181-186
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    • 2005
  • This experiment was conducted to know the appropriate methods for extraction and determination of rutin contained buckwheat plants. The efficient HPLC analytical condition of rutin contained buckwheat plants was developed. The gradient elution employed a $250mm\times4.6mm$ i.d. Tosoh ODS 120T column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of $2\%$ Acetic $acid-45\%$ Acetonitrile, and mobile phase B, comprising $2\%$ aqueous acetic acid, and delivered at a flow rate of 1mL/min as follows: 0-18 min, $50-100\%$ A; 18-20 min, $100-50\%$ A; 20-22 min, $50\%$ A. The UV detection wavelength was set at 355 nm. The limit of detection (LOD) for rutin standard compound was 20 ng/mL. And, the higher content of rutin in the extracts was obtained by $80^{\circ}C$ reflex extraction for 120 min. from plants of buckwheat using ethanol.