• Title/Summary/Keyword: liquid column separation

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Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

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.

Simultaneous Determination of Penicillin Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 페니실린계 항생제 8종의 동시분석 및 적용성 검증)

  • Kim, Myeong-Ae;Yoon, Su-Jin;Kim, MeeKyung;Cho, Yoon-Jae;Choi, Sun-Ju;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.131-140
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    • 2014
  • The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).