• Title/Summary/Keyword: Analytical Chromatography

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Contents of vitamin B9 (folate) and B12 (cobalamins) in commonly consumed seafood menus in Korea (한국인 상용 수산물 식단의 비타민 B9과 B12 함량)

  • Park, Eun-Young;Jeong, Bomi;Chun, Jiyeon
    • Journal of Nutrition and Health
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    • v.54 no.2
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    • pp.211-223
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    • 2021
  • Purpose: A total of 39 seafood menus were prepared according to the Korean standard recipe, and analyzed for vitamin B9 (folate) and B12 (cobalamins) contents, using validated applied analytical methods. The menus included Guk/Tang/Jjigae (boiled or stewed dishes, n = 10), Bokkeum (stir-fried dishes, n = 10), Jjim/Jorim (braised or steamed dishes, n = 7), Gui (baked or grilled dishes, n = 7), Twigim (deep-fried dishes, n = 2) and Muchim (dried or blanched-seasoned dishes, n = 3). Methods: The contents of vitamin B9 and B12 in all food samples were determined by the trienzyme extraction-Lactobacillus casei and immunoaffinity-high-performance liquid chromatography/photodiode array detection methods. Analytical quality control was performed in order to assure reliability of the analysis. Results: Accuracy (97.4-100.6% recoveries) and precision (< 6% relative standard deviations for repeatability and reproducibility) of vitamin B9 and B12 analyses were determined to be excellent. The vitamin B9 and B12 contents of the 39 seafood menus evaluated, varied in the range of 1.83-523.08 ㎍/100 g and 0.11-38.30 ㎍/100 g, respectively, depending on the ingredients and cooking methods. The vitamin B9 content was highest in Jomi-gim (523.08 ㎍/100 g), followed by Geonsaeu-bokkeum (128.34 ㎍/100 g) and Janmyeolchi-bokkeum (121.53 ㎍/100 g). Vitamin B12 was detected in all seafood menus, with highest level obtained in Kkomack-jjim (41.58 ㎍/100 g). The seaweed dish was found to have high levels of both vitamin B9 and B12. All assays were performed under strict quality control. Conclusion: Guk and Tang menus, which contain a large amount of water, were relatively lower in the vitamin B9 and B12 contents than the other menus. Bokkeum menus containing various vegetables were high in the vitamin B9 content, but the vitamin B12 content was dependent on the type of seafood used in the menu.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Studies on Xylooligosaccharide Analysis Method Standardization using HPLC-UVD in Health Functional Food (건강기능식품에서 HPLC-UVD를 이용한 자일로올리고당 시험법의 표준화 연구)

  • Se-Yun Lee;Hee-Sun Jeong;Kyu-Heon Kim;Mi-Young Lee;Jung-Ho Choi;Jeong-Sun Ahn;Kwang-Il Kwon;Hye-Young Lee
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.72-82
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    • 2024
  • This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C18 column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

Analysis of Water Soluble Vitamin B1, B2, and B3 Contents in Korean Traditional Holiday Foods (우리나라 명절 및 제사음식에 함유된 수용성 비타민 B1, B2 및 B3의 함량 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.8
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    • pp.944-951
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    • 2017
  • This study aimed to determine and examine the contents of vitamins $B_1$, $B_2$, and $B_3$ using the high-performance liquid chromatography method in traditional holiday foods in Korea. All analyses were under the quality control chart of vitamins $B_1$, $B_2$, and $B_3$. The z-scores for vitamins $B_1$, $B_2$, and $B_3$ were 1.3, 0.0, and 0.6, respectively, in food analysis performance assessment scheme proficiency tests assuring reliability of analytical performance. Vitamin $B_1$, $B_2$, and $B_3$ contents were analyzed in a total of 31 samples. Vitamin $B_1$, $B_2$, and $B_3$ contents ranged from 0.000 to 0.973 mg/100 g, from 0.037 to 0.264 mg/100 g, and from 0.000 to 1.223 mg/100 g in Korean traditional holiday foods, respectively. The highest contents of vitamins $B_1$, $B_2$, and $B_3$ were 0.973 mg/100 g in Yukwon-jeon, 0.264 mg/100 g in Dongtae-jeon, and 1.223 mg/100 g in Yukwon-jeon sample, respectively. However, compared to vitamins $B_2$ and $B_3$, vitamin $B_1$ was not detected, generally. Therefore, these results can be used as basic data for a food composition table and improvement of national health for Koreans.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

tans-Resveratrol Content of Varieties and Growth Period in Peanut (땅콩 품종 및 생육기별 trans-Resveratrol 함량)

  • Lee, Mi-Ja;Cheong, Young-Keun;Kim, Hyung-Soon;Park, Ki-Hun;Doo, Hong-Soo;Suh, Duck-Yong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.48 no.6
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    • pp.429-433
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    • 2003
  • trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

Determination of β-Carotene and Retinol in Korean Noodles and Bread Products (가공 및 외식식품 중 면류 및 제빵류의 레티놀 및 베타카로틴 함량 조사)

  • Shin, Jung-Ah;Chun, Ji Yeon;Lee, Junsoo;Shin, Ki Yong;Lee, Soon Kyu;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.12
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    • pp.1949-1957
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    • 2013
  • The contents of ${\beta}$-carotene and retinol in processed and restaurant foods, such as Korean noodles, mandus, rice cakes and bread products, were quantified by high-performance liquid chromatography (HPLC) with UV/visible and fluorescence detector, respectively. Samples were collected from different local areas (i.e. Gangwon-do, Gyeonggi-do, Gyeongsang-do, Seoul, Jeolla-do, and Chungcheong-do). After homogenization, samples were hydrolyzed by direct alkali saponification; thereafter, fat-soluble components were extracted by a mixture of n-hexane/ethylacetate (85:15, v/v), containing 0.01% butylated hydroxytoluene (BHT). ${\beta}$-carotene and retinol contents in infant formula used as an in-house material for the analytical quality control. Among 14 Korean noodles, high contents of ${\beta}$-carotene were found in Bibim-Guksu (average 442.43 ${\mu}g/100g$) and Jjolmyeon (average 301.39 ${\mu}g/100g$). In 4 Korean mandus, the highest contents of ${\beta}$-carotene was determined in Kimchi-mandu (average 197.64 ${\mu}g/100g$), resulting in 33.3 RE of the converted vitamin A. Among 12 Korean rice cakes, Maeun-Tteokbokki and Modm-Chaltteok contained relatively high content of ${\beta}$-carotene with 205.11 and 41.33 ${\mu}g/100g$, respectively, while retinol was detected only in Maeun- Tteokbokki (1.65~10.45 ${\mu}g/100g$). In addition, among 8 bread products, 77.3 RE of pastry, 51.2 RE of buttercream- bread, and 41.4 RE of morning roll were found as the contents of the converted vitamin A.

A Simultaneously Analytical Method of Phthalate and Adipate Plasticizers in Food Packaging by Dual-Column GC-FID System (Dual-Column GC-FID System을 이용한 식품 포장재 중 Phthalate류 및 Adipate류 가소제의 동시 분석법)

  • Kang Gil-Jin;Kwak In-Shin;Eom Mi-Ok;Jeon Dea-Hoon;Kim Hyung-il;Sung Jun-Hyun;Choi Jung-Mi;Kim Eun-Kyung;Lee Young Ja
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.277-283
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    • 2005
  • A plasticizer is a substance which is added to a material to improve its processability, flexibility and stratchability. Phthalates and adipates are the most frequently used plasticizers of poly(vinyl chloride) (PVC). However, they can migtate into food from PVC food packaging, and some of them are especially suspected as endocrine disruptors. In this study, Simultaneous analysis of 13 phthalates and 9 adipates were carried out by dual-column gas chromatography system equipped wi two FID detectors for rapid confirmation and quantification. The Proposed method was validated with > 0.993 of linearity in the ranges of 10-500 mg/l, < $3.5\%$ RSD of reproducability in 10 inter-days sample preparations, and > $98.1\%$ of recoveries for all the plasticizers. DEHA was detected in all the 3 PVC wraps at levels of 176.9-198.5mg/g. Among the 51 samples of PVC gaskets, the targeted plasticizers were detected in 41 samples. Of these plasticizer detected samples,40 contained DIDP at the levels of 157.3-374.7 mg/g and one contained DMP at the levels of 165.6 mg/g. Also, some plasticizers were detected in other packaging materials such as PET, PP, PE, Pulp. But it might be attributed to contamination in manufacturing.

A Study on the Analytical Method of Artificial Sweeteners in Foods (식품 중 인공감미료의 분석법에 관한 연구)

  • Kim, Hee-Yun;Yoon, Hae-Jung;Hong, Ki-Hyung;Lee, Chang-Hee;Park, Sung-Kwan;Choi, Jang-Duck;Choi, Woo-Jeong;Park, Sun-Young;Kim, Ji-Hye;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.36 no.1
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    • pp.14-18
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    • 2004
  • Analysis methods of artificial sweeteners, aspartame, acesulfame potassium, sodium saccharin, and sucralose isolated from foods were developed using high performance liquid chromatography, HPLC conditions for aspartame, acesulfame potassium, and sodium saccharin were: column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, 0.05M sodium phosphate monobasic : acetonitrile (9 : 1, pH 3.5, containing 0.01M tetrapropylammonium hydroxide); detector, UV detector at 210 nm. HPLC condition for sucralose were : column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, water:methanol (7 : 3); detector, refractive index detection (sensitivity = 16). Recoveries of artificial sweeteners in foods including soft drinks, fruit and vegetable beverages, alcoholic beverages, fermented milk beverages, soybean milk, ice cream, snacks, chewing gums, jam, honey, kimchi salted food, special dietary products, processed fish products, candies, food additive mixtures, chocolate and cocoa were 76.1-101.3%, 82.3-103.2%, 83.1-103.7%, and 80,6-99.5% for aspartame, acesulfame potassium, sodium saccharin, and sucralose, respectively.

Development of a Residue Analysis Method for Metamifop in Paddy Water, Soil, and Rice with HPLC (HPLC를 이용한 농업용수, 논토양, 및 현미 중 metamifop의 잔류분석법 개발)

  • Park, Hee-Woon;Moon, Joon-Kwan
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.68-74
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    • 2017
  • An analytical method for detecting metamifop residue in paddy water, soil, and rice with high performance liquid chromatography (HPLC) was developed. Water was extracted with ethyl acetate before analyzing by HPLC. Soil residues were extracted with acetone under acidic condition and after purifying with $Extrelut^{(R)}$ NT, and silica SPE, the residue was analyzed by HPLC. For residue analysis in rice, the procedure involved extraction with acetone, purification with $Extrelut^{(R)}$ NT, partitioning between acetonitrile/hexane, purification with silica SPE cartridge, and analysis by HPLC. The limit of detection (LOD) was 1.0 ng, limit of quantitation (LOQ) was 3.0 ng, and method limit of quantitation (MLOQ) were 0.001 mg/L for paddy water, 0.01 mg/kg for rice and soil, respectively. Standard calibration curve shows linearity from 0.05 mg/kg to 5.0 mg/kg ($R^2=0.9999$). The recoveries in fortified paddy water were $91.3{\pm}3.5%$ (0.01 mg/L level) and $93.2{\pm}6.3%$ (0.05 mg/L level). The recoveries in fortified paddy soils were $92.5{\pm}4.0%$ (0.1 mg/kg level) and $92.7{\pm}4.0%$ (0.5 mg/kg level) in soil A, while, $102.3{\pm}4.4%$ (0.1 mg/kg level) and $98.9{\pm}7.9%$ (0.5 mg/kg level) in soil B, respectively. The recoveries in fortified rice were $93.0{\pm}6.9%$ (0.1 mg/kg level) and $85.0{\pm}3.5%$ (0.5 mg/kg level). This method was proved to be effective and can be used to determine the metamifop residue in paddy water, paddy soil, and rice.