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A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS (HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구)

  • Lee, Seong-Bong;Yong, Kum-Chan;Hwang, Sun-Il;Kim, Young-Su;Jung, You-Jung;Seo, Mi-Young;Lee, Chang-Hee;Sung, Jin-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.327-333
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    • 2014
  • A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

Studies on the Determination Method of Monascus Pigments in Foods (식품 중 홍국색소의 분석법에 관한 연구)

  • Lee, Tal-Soo;Lee, Young-Ja;Kwon, Yong-Kwan;Park, Jae-Seok;Ko, Hyun-Sook;Sim, Kyu-Chang;Lee, Ju-Yeun;Shin, Jae-Wook;Song, Jee-Won;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.33 no.5
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    • pp.641-644
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    • 2001
  • This study was performed for development of new analytical method of monascus pigments in foods. In this method, analysis of monascus pigment in foods has been carried out by detection of monascin and ankaflavin of the main color component of monascus pigment as indicator compounds. Monascin and ankaflavin were isolated and identified by TLC, HPLC, Prep. HPLC, $^{1}H-NMR$ and Mass spectrophotometer. The analysis of monascin and ankaflavin in foods such as massal, sausage, mixed press ham, mixed fish sausage, semi-dried sausage and syrup was performed by using reverse phase high performance liquid chromatograph with Capcell Pak C18 column at wave length 390 nm. The quantitative results of monascin were as follows : $0.01{\sim}3.31\;{\mu}g/g$ item in massal, $0.05{\sim}0.10\;{\mu}g/g$ in mixed fish sausage, and $0.34{\sim}0.35\;{\mu}g/g$ in semi-dried sausage. But the quantitative results of ankaflavin were as follows: $0.02{\sim}0.89\;{\mu}g/g$ in massal, ankaflavin were not founded in other samples.

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LC-MS/MS analysis and anti-inflammatory effects of crude extract from Coptidis Rhizoma (황련 추출물의 LC-MS/MS 분석 및 항염증 효과)

  • Min-Jung, Kim;Ye-Jin, Yang;Kwang-Youn, Kim;Hun Hwan, Kim;Jae Dong, Son;Ju-Hye, Yang;Dong bin, Lee;Woo Hyun, Kim;Hu-Jang, Lee;Seon Been, Bak;Kwang-Il, Park
    • Herbal Formula Science
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    • v.31 no.1
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    • pp.1-10
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    • 2023
  • Objectives : The main aim of this study was to examine the LC-MS/MS used to identify phenolic compounds of CRE(Coptidis Rhizoma 70% EtOH Extract). Also, we investigated antioxidative activities and Anti-inflammatory activities. Methods : LC-MS/MS Analysis HPLC and LC-MS/MS were performed on a 1260 series HPLC system (Agilent Technologies, Inc., California, USA) and 3200 QTrap tandem mass system (Sciex LLC) operated in positive ion mode (spray voltage set at -4.5 kV). The solvent used was DW and Acetonitrile containing 0.1% formic acid, a gradient system was used at a flow rate of 0.5 mL/min for analysis, and a Prontosil C18 column (length, 250 mm; inner diameter, 4.6 mm; particle size, 5 ㎛; Phenomenex Co., Ltd., California, USA, Biochoff Chromatography) was used. The solvent conditions used in the mobile phases were 0-10 min at 10-15% B, 10-20 min at 20% B, 20-30 min at 25%, 30-40 min at 40%, 40-50 min at 70%, 50-60 min at 95%, and 60-70 min at 95%. The analysis was performed at a wavelength of 284 nm and a temperature of 35℃. The cell viability was measured using a 3-(4,5-dimethyethiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity. We examined the effects of CRE on the lipopolysaccharide (LPS)-induced production of nitric oxide (NO) in a RAW 264.7 cells Results : The chemical analysis CRE by Liquid chromatography-tandem mass spectrometry (LC-MS/MS) confirmed that Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid as phenolic components. DPPH radical scavenging activity was the inhibitory activity of CRE showed at 200 ㎍/mL a statistically significant level. MTT assay demonstrated that the CRE did not have a cytotoxic effect in RAW 264.7 and LPS-induced RAW264.7 cells. Also, CRE reduced NO production in RAW 264.7 cells stimulated with LPS. Conclusions : Based on these findings, The chemical analysis 4 major components CRE such as Rosmarinic acid, Ferrulic acid, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid. Moreover, we confirmed that CRE has effects antioxidant and anti-inflammatory. The results demonstrate that CRE can be used as an antioxidant and a powerful chemopreventive ingredient against inflammatory diseases.

Comparative Studies on the Lipid Composition in Varieties of Dent Corn (마치종(馬齒種)옥수수의 품종별(品種別) 지질조성(脂質組成)의 비교(比較))

  • Ahn, Doo-Hee;Ha, Bong-Seuk
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.16 no.4
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    • pp.350-363
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    • 1987
  • This study dealt with the comparison of the individual lipid component and fatty acid composition in the six varieties of dent corn, Zea mays Indentata. The fatty acid and sterol compositions of the total lipid were analyzed by gas liquid chromatography. The total lipid was also fractionated into three lipid classes namely neutral, glyco and phospolipid by the methods of silicic acid column chromatography. The lipid componets of lipid-classes were estimated by thin layer chromatography and TLC-scanner. The contents of total lipid in six varieties of Cdent corn were $3.7{\sim}5.3%$. Total lipid were mainly Composed of triglyceride$(69.8{\sim}75.7%)$ free fatty acid$(13.0{\sim}17.9%)$, lanosterol$(4.8{\sim}6.0%)$. hydrocarbon & esterified sterol$(3.5{\sim}6.0%)$, and polar lipid & pigment$(2.7{\sim}5.9%)$. The contents of triglycerde in $Chech'{\breve{o}}nok$ and Hwangok No.3 were slightly higher then other varieties. The major fatty acid In total lipid from six varieties of dent corn were chiefly consisted of linoleic$(46.0{\sim}61.4%)$, oleic$(21.9{\sim}29.9%)$ and palmitic acid$(10.9{\sim}16.7%)$. Particularly the content of linoleic acid in $Chech'{\breve{o}}nok$ was higher but oleic and palmitic acid in $Chech'{\breve{o}}nok$ were less than other varieties. The compositions of 4-desmethylsterol were mainly composed of siterol $(44.0{\sim}63.2%)$, campestetel$(11.6{\sim}15.5%)$ and stigmasterol$(5.6{\sim}9.1%)$. The content of sitosterol in Chinjuok was higher than other varieties and isofucosterol was detected only in Chinjuok. The compositions of 4-monomethlysterol were mainly composed of obtusifoliol$(17.7{\sim}37.6%)$, gramisterol$(15.0{\sim}27.0%)$ and citrostadienol$(9.1{\sim}17.3%)$. The contents of obtusifoliol and citrostadienol in Kwangok and Chinjuok were less than other varieties. The contents of fractionated neural lipid in Suwon No.19. Kwangok, $Hoengs{\breve{o}}ngok$ and Chinjuok$(90.3{\sim}97.1%)$ were higher than those of $Chech'{\breve{o}}nok$ and Hwangok No.3$(85.5{\sim}86.1%)$. Neutral lipid were mainly composed of triglyceride$(24.7{\sim}80.0%)$, lanosterol$(6.2{\sim}20.2%)$, Cholesterol$(1.0{\sim}50.6%)$, free fatty acid$(4.4{\sim}8.9%)$ and esterified sterol$(1.5{\sim}15.9%)$. The major fatty acid in neutral lipid from six varieties of dent corn were chiefly consisted of linoleic$(26.2{\sim}55.4%)$ oleic$(22.7{\sim}39.1%)$ and palmitic acid$(11.4{\sim}41.6%)$. Particularly the contents of linoleic acid Suwon No.19 and $Chech'{\breve{o}}nok$ were higher but palmtic acid in Suwon No.19 and $Chech'{\breve{o}}nok$ were less tan other varieties. Glycolipd were mainly composed of nlonoglycosflsterol $(17.5{\sim}56.4%)$, monoglycosylce-ramide $(8.2{\sim}25.9%)$ and monoglycoslydiacylglycerol$(12.4{\sim}22.2%)$. The contents of mono-g1ycosrlceramide and monoglycosrlsterol in Chinjuok. Were higher than other varieties. The major fatty acid in glycolipid from six varieties of dent corn were chiefly consisted$(14.6{\sim}39.3%)$, palmitic$(20.0{\sim}26.1%)$, linoleic$(3.6{\sim}26.9%)$ and heptadecanoic acid $(3.3{\sim}24.7%)$. Particutarly the cantents of oleic acid in Chinjuok and heptadecanoic acid in $Chech'{\breve{o}}nok$ were higher than other varieties. Phospholipid were mainly composed of phosphatidyllnositol$(30.9{\sim}86.4%)$ and phosphatidylcholine$(4.5{\sim}22.0%)$. The contents of phosphatidrlinositol in $Hoengs{\breve{o}}ngok$ and Hwanngok No. 3 were less than other varieties. The major fatty acid in phospolipid from six varieties of dent corn chiefly consisted of patmitic$(37.2{\sim}61.6%)$ heptadecanoic$(9.2{\sim}31.8%)$ and oleic acid$(4.3{\sim}17.2%)$. Particuiarlr the content of oleic acid in $Hoengs{\breve{o}}ngok$ was higher but heptadccanoic acid in $Hoengs{\breve{o}}ngok$ was less than othcr varieties.

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Studios on Lipids in Fresh-Water Fishes 5. Distribution of Lipid Components in Various Tissues of Carp, Cyprynus carpio (담수어의 지질에 관한 연구 5. 잉어(Cyprynus carpio)의 부위별 지질성분의 분포)

  • CHOI Jin-Ho;RO Jae-Il;BYUN Dae-Seok;PYEUN Jae-Hyeung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.18 no.2
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    • pp.149-156
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    • 1985
  • Distribution of lipid components in the tissue of meat, skin and viscera from carp(Cyprynus carpio) was analyzed using the techniques of column chromatography, thin layer chromatography and gas liquid chromatography according to the previous report(Choi, et al., 1984). Lipid content was varied by the portion such as $3.88\%$ in meat (free lipid, $2.47\%$ ; bound lipid, $1.41\%$), $8.02\%$ in skin(free lipid, $5.65\%$ ; bound lipid, $2.37\%$) and $6.18\%$ in viscera (free lipid, $3.54\%$ ; bound lipid, $2.64\%$). In the all portions of the body, free lipid was composed of $68\%\;to\;92\%$ in neutral lipid, $3\%\;to\;6\%$ in glycolipid and $4\%\;to\;18\%$ in phospholipid whereas bound lipid was composed of $8\%\;to\;20\%$ in neutral lipid, $2\%\;to\;7\%$ in glycolipid and $47\%\;to\;62\%$ in phospholipid. The free lipids of the tissues on the each portion were mostly represented by triglycerides and some diglycerides, but free lipids in viscera contained considerable amounts of free fatty acids. The bound lipids, on the other hand, commonly comprised appreciable amounts of esterified sterol and hydrocarbon, and triglycerides. The phospholipid was mainly consisted of phosphatidyl choline, phosphatidyl ethanolamine and phosphatidyl serine in the both free and bound lipids, and much more phosphatidyl choline in the bound lipid. The predominant fatty acids of free and bound lipids were $C_{16:0},\;C_{18:0},\;C_{20:4},\;C_{22:6}\;and\;C_{18:2}$ acids in polar lipids, and $C_{16:0},\;C_{16:1},\;C_{18:0},\;C_{18:1}\;and\;C_{18:2}$ acids in non-polar lipids, whereas those of neutral lipids were $C_{14:0}(2.54{\sim}6.98\%),\;C_{16:0}(11.20{\sim}21.13\%)$ and $C_{18:0}(1.58{\sim}12.76\%)$ of saturated acids, $C_{16:1}(7.06{\sim}20.70\%),\;C_{18:1}(21.68{\sim}30.50\%)$ and $C_{20:1}(1.76{\sim}6.27\%)$ of monoenoic acids, and $C_{18:2}(4.50{\sim}6.89\%),\;C_{20:4}(1.52{\sim}4.29\%)$ and $C_{22:6}(0.73{\sim}6.62\%)$, respectively. In conclusion, the fatty acid compositions revealed apparent differences between the free lipid and bound lipids in the tissues of body.

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