• Title/Summary/Keyword: RSD

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Analysis of ITX from Commercial Carton Packs in Korean Market (국내 유통 종이팩 포장재 중 Isopropylthioxanthone(ITX) 분석)

  • Eom, Mi-Ok;Yoon, Hae-Jung;Choi, Hyun-Cheol;Jeon, Dae-Hoon;Kim, Hyung-Il;Sung, Jun-Hyun;Park, Na-Young;Lee, Eun-Joon;Sung, Duk-Hwa;Lee, Young-Ja
    • Journal of Food Hygiene and Safety
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    • v.22 no.2
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    • pp.88-92
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    • 2007
  • Isopropylthioxanthone(ITX) is used as a photoinitiator In UV-cured inks, triggering the radical polymerization of the acrylic component of such inks and thus causing the liquid ink film to cure. Recently ITX was detected in carton packed food in Italy. In order to cope with risk issues of overseas and acquire monitoring data on ITX, we have established the method using HPLC/FLD for ITX analysis after reviewing parameters of the analytical methods. Limit of detection (LOD) and limit of quantification (LOQ) were 0.02 ppb and 0.1 ppb, and linearity and RSD (%) were 0.9991 and 1.09, respectively. We have investigated ITX levels migrated to food on 87 commercial products packed in carton and ITX was not detected any food. Therefore it is supposed that UV-cured ink containing ITX as photoinitiator is not currently used in printing of carton pack in Korea.

Development of Analytical Methods of Hyperoside from Rosa canina L. (Rosa canina L. 중 hyperoside의 시험법 개발 연구)

  • Oh, Jae Myoung;Lee, Hwa Jung;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Park, Ji Min;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.173-177
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    • 2015
  • Rosa canina L. is health functional food materials that can help to temporarily relieve symptoms of arthritis. This study has been conducted to develop and validate analytical methods for hyperoside of Rosa canina L.. Methods based on HPLC with ultraviolet detection (UVD) were established through instrumental analytical conditions, and the examination of data, such as domestic and foreign reliable methods and journals. HPLC UVD analysis using Capcell Pak C18 MG II column at 353 nm was determined on test through the column, mobile phase. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for hyperoside. The method showed high linearity in the calibration curve at a coefficient of correlation (R2) of 0.999, and the LOQ was 0.393μg/mL. Relative standard deviation (RSD) values of data from repeatability precision was between 0.6 and 2.6%. Recovery rate test at hyperoside scored between 98 and 99%. These results indicate that the established HPLC method is very useful for the determination of hyperoside in Rosa canina L. to develop a health functional material.

Determination of Ethylenethiourea in Fruits (과실류에 잔류하는 Ethylenethiourea 분석)

  • Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
    • Korean Journal of Food Science and Technology
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    • v.43 no.3
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    • pp.277-281
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    • 2011
  • A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were 73.6μg/kg and 29.8μg/kg.

Anaylsis of γ-aminobutyric Acid (GABA) Content in Germinated Pigmented Rice (발아 유색미의 GABA(γ-aminobutyric acid) 함량 분석)

  • An, Mi-Kyoung;Ahn, Jun-Bae;Lee, Sang-Hwa;Lee, Kwang-Geun
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.632-636
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    • 2010
  • The level of γ-aminobutyric acid (GABA) in pigmented rice was quantitatively and qualitatively determined by high pressure liquid chromatography/fluorescence detection (HPLC/FLD). In this study, the recovery rate and limit of detection (LOD) of GABA were 122.4±2.4% and 0.23 μg/g, respectively. The geminating pigmented rice samples, which were harvested in Paju, Korea, were soaked in water at 18C for 20 hr. After soaking, the samples were germinated at 30C for about 24 hr. GABA content was highest (293.0 μg/g) in the germinated red rice. Furthermore, GABA levels in the germinated rice increased significantly by up to 11.1 and 24.7-fold as compared to non-germinated rice and milled rice, respectively. The GABA concentrations of non-germinated rice, with the exception of red rice, were significantly higher than those of milled rice by 7.6-20.6-fold.

Determination of Post-harvest Fungicide in Citrus Fruits Using LC-MS (LC-MS를 이용한 감귤류의 수확 후 처리 살균제 분석)

  • Choi, Su-Jeong;Kim, Eun-Jeong;Lee, Jae-In;Cho, In-Soon;Park, Won-Hee;Hwang, In-Sook;Kim, Moo-Sang;Kim, Gun-Hee
    • Korean Journal of Food Science and Technology
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    • v.45 no.4
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    • pp.409-415
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    • 2013
  • Post-harvest fungicide residue was measured in citrus fruits. Samples were collected from local markets in Seoul and analyzed using liquid chromatography coupled with mass spectrometry (LC-MS). LC-MS results were validated for the assay of pesticides by using linearity, accuracy, precision, and limits of detection and quantification. The linearity in the concentration ranged from 0.005 to 2.0 mg/kg (R2 >0.999). Sample recoveries ranged from 80.2 to 98.3% with relative standard deviations below 4.0% for spiking levels from 0.01 to 1.0 mg/kg. The limits of detection ranged between 0.002 and 0.008 mg/kg, and the limits of quantification ranged between 0.006 and 0.027 mg/kg. The highest residue levels for carbendazim, thiabendazole, imazalil, and azoxystrobin in citrus fruits were 0.541, 0.958, 0.721, and 0.052 mg/kg, respectively. The pesticide residues found in citrus fruits were blow maximum residue limits (MRLs) and are not a serious public health problem.

Development and Validation of a Simultaneous Analytical Method for the Detection of Mefentrifluconazole and Triticonazole Fungicide in Agricultural Crops (농산물 중 메펜트리플루코나졸 및 트리티코나졸 살균제의 동시 분석법 개발 및 검증)

  • Park, Ji-Su;Lee, Han Sol;Lee, Su Jung;Shin, Hye-Sun;Shim, Jae-Han;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Korean Journal of Environmental Agriculture
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    • v.39 no.2
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    • pp.130-137
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    • 2020
  • BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r2>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

Method Development for Determination of Trichothecene Mycotoxins in Nuts by LC-MS/MS (LC-MS/MS를 이용한 견과류 중 트리코테센계 곰팡이 독소 10종 동시분석법 개발)

  • Kim, Dan-Bi;Park, Ji-Su;Yoo, Mi-Young
    • Journal of Food Hygiene and Safety
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    • v.33 no.5
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    • pp.354-360
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    • 2018
  • This study presents a method validation for extraction and quantitative analysis of trichothecene mycotoxins in nuts based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach for extraction and enhanced matrix removal (EMR)-lipid-disperive-SPE (d-SPE) cleanup method, with detection and quantification by high-performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) in positive- and negative-ion modes. Linearity, precision, and accuracy were validated for LC-MS/MS methods. Results obtained with LC-MS/MS were linear, with correlation coefficient (R2) of 0.998. Limits of detection and quantification for mycotoxins were 0.413.57μg/kg and 1.2310.82μg/kg, respectively. Intra- and inter-day precisions (RSD, %) were 0.40-8.44% and 1.93-12.46%, respectively. Results indicated to be rapidly and accurately identifying trichothecene mycotoxins and may be used as a suitable safety management method for nuts and nuts related commodities.

Extraction and Preprocessing Methods for Ginsenosides Analysis of Panax ginseng C.A. Mayer (인삼의 진세노사이드 분석을 위한 추출 및 전처리법)

  • Kim, Geum-Soog;Hyun, Dong-Yun;Kim, Young-Ock;Lee, Sung-Woo;Kim, Young-Chang;Lee, Seung-Eun;Son, Yeong-Deck;Lee, Min-Jeong;Park, Chung-Berm;Park, Ho-Ki;Cha, Seon-Woo;Song, Kyung-Sik
    • Korean Journal of Medicinal Crop Science
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    • v.16 no.6
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    • pp.446-454
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    • 2008
  • An advanced extraction method by ultrasonic extraction with applied solid phase extraction (SPE) has been developed for the determination of simultaneous eight major ginsenosides, namely ginsenosides Rg1, Re, Rf, Rb1, Rg2, Rc, Rb2, and Rd in the root of Panax ginseng. Four extraction methods including n-BuOH reflux extraction (Method A), 70% EtOH reflux extraction (Method B), 50% MeOH reflux extraction with SPE (Method C), and 50% MeOH ultrasonication with SPE clean-up process (Method D) were investigated for the determination of eight major ginsenosides. Total contents of ginsenosides were highest by extraction of Method C as 2.408±0.011. However, Method D was evaluated as relatively simpler and more efficient method due to short extraction time, small solvent consumption and less expensive, compared to conservative reflux method. Ginsenosides were also satisfactorily separated with good resolution and the accuracy range was between 1.05 and 4.06% as relative standard deviation (RSD) by Method D. SPE condition and HPLC condition were further optimized for determination of eight major ginsenosides by the ultrasonic extraction method. Conclusively, ultrasonic extraction of 2 g sample of ginseng using ultrasonic bath and 1 loading for SPE was evaluated as proper condition for extraction of ginseng.

A Study on Standardization of Shinbaro Pharmacopuncture Using Herbal Medicines Identification Test and HPLC-DAD (신바로 약침의 한약재 확인시험 및 HPLC-DAD를 통한 표준화 연구)

  • Lee, Jin Ho;Kim, Min Jeong;Lee, Jae Woong;Kim, Me Riong;Lee, In Hee;Kim, Eun Jee
    • Journal of Acupuncture Research
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    • v.32 no.2
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    • pp.1-9
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    • 2015
  • Objectives : The present study was an evaluation and standardization of herbal components in order to establish the efficacy and safety of Shinbaro pharmacopuncture. Methods : Among the raw materials of Shinbaro pharmacopuncture, the components Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix were assessed through ingredient verification experiments using thin-layer chromatography(TLC) and ultraviolet rays(UV) lamps. In addition, we standardized Acanthopanacis Cortex and Achyranthis Radix through validation using high performance liquid chromatograph-diode array detector(HPLC-DAD). Results : As result appeared a blue-white fluorescence under ultraviolet rays; changed to dark green after adding 1 % ferric chloride solution(due to Cibotii Rhizoma), and presented a yellow-green fluorescence when mixed with an ethyl ether under UV lamps by way of the ethyl ether layer, confirming Eucommiae Cortex. Ledebouriellae Radix was confirmed as dark brown spots at Rf values of 0.56 and 0.71 using TLC. Additionally, Acanthopanacis Cortex and Achyranthis Radix HPLC test results showed that linearity was R20.99, and detection limit and quantitation limit were 0.23 to 1.29μg/mL, and 0.71 to 3.90μg/mL, respectively. Furthermore, precision and accuracy were confirmed to have relative standard deviation(RSD) values of 0.10 to 1.89 % and 96.19 to 103.72 %, respectively. Shinbaro pharmacopuncture did not have any overlapping or interference from other peaks in detection under the abovementioned analysis conditions. Conclusions : In conclusion, we confirmed that maintenance of Shinbaro pharmacopuncture validity was possible by means of quality control of Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix through ingredient identification and Acanthopanacis Cortex and Achyranthis Radix through high performance liquid chromatograph(HPLC) analysis. Further, we hope to contribute to the development strategy of herbal industry acupuncture.

Pattern Recognition of the Herbal Drug, Magnoliae Flos According to their Essential Oil Components

  • Jeong, Eun-Sook;Choi, Kyu-Yeol;Kim, Sun-Chun;Son, In-Seop;Cho, Hwang-Eui;Ahn, Su-Youn;Woo, Mi-Hee;Hong, Jin-Tae;Moon, Dong-Cheul
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1121-1126
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    • 2009
  • This paper describes a pattern recognition method of Magnoliae flos based on a gas chromatographic/mass spectrometric (GC/MS) analysis of the essential oil components. The botanical drug is mainly comprised of the four magnolia species (M. denudata, M. biondii, M. kobus, and M. liliflora) in Korea, although some other species are also being dealt with the drug. The GC/MS separation of the volatile components, which was extracted by the simultaneous distillation and extraction (SDE), was performed on a carbowax column (supelcowax 10; 30 m{\time}0.25 mm{\time}0.25{\mu}m$) using temperature programming. Variance in the retention times for all peaks of interests was within RSD 2% for repeated analyses (n = 9). Of the 74 essential oil components identified from the magnolia species, approximately 10 major components, which is α-pinene, β-pinene, sabinene, myrcene, d-limonene, eucarlyptol (1,8-cineol), γ-terpinene, p-cymene, linalool, α-terpineol, were commonly present in the four species. For statistical analysis, the original dataset was reduced to the 13 variables by Fisher criterion and factor analysis (FA). The essential oil patterns were processed by means of the multivariate statistical analysis including hierarchical cluster analysis (HCA), principal component analysis (PCA) and discriminant analysis (DA). All samples were divided into four groups with three principal components by PCA and according to the plant origins by HCA. Thirty-three samples (23 training sets and 10 test samples to be assessed) were correctly classified into the four groups predicted by PCA. This method would provide a practical strategy for assessing the authenticity or quality of the well-known herbal drug, Magnoliae flos.