• Title/Summary/Keyword: code validation

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Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Analytical Method for Sodium Polyacrylate in Processed Food Products by Using Size-exclusion Chromatography (Size-exclusion Chromatography를 활용한 가공식품 중 폴리아크릴산나트륨 분석법 확립)

  • Jeong, Eun-Jeong;Choi, Yoo-Jeong;Lee, Gunyoung;Yun, Sang Soon;Lim, Ho Soo;Kim, MeeKyung;Kim, Yong-Suk
    • Journal of Food Hygiene and Safety
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    • v.33 no.6
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    • pp.466-473
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    • 2018
  • An analytical method of sodium polyacrylate in processed food products was developed and monitored by using size-exclusion chromatography. GF-7M HQ column and UV/VIS detector were selected based on peak shape and linearity. Flow rate, column oven temperature, and mobile phase were selected as 0.6 mL/min, $45^{\circ}C$, and 50 mM sodium phosphate buffer of pH 9.0, respectively. Samples for analysis of sodium polyacrylate were extracted with 50 mM sodium phosphate buffer of pH 7.0 for 3 hr at $20^{\circ}C$ and 150 rpm. Analytical method validation revealed proper selectivity and calibration curve was selected in the range of 50-500 mg/L, and correlation coefficient of calibration curve was more than 0.9985. Limit of detection of sodium polyacrylate was 10.95 mg/kg and limit of quantification was 33.19 mg/kg. Accuracy and coefficient of variation for sodium polyacrylate analysis was 99.6-127.6%, 3.0-8.3% for intra-day and 94.3-121.9%, 1.3-2.6% for inter-day, respectively. Sodium polyacrylate was detected in 40 samples among monitored 125 processed food products. Detected contents were less than 0.2%, limited by the Food Additives Code. Results suggest the established size-exclusion chromatography method could be used to analyze sodium polyacrylate in processed food products.

Optimization and Applicability Verification of Simultaneous Chlorogenic acid and Caffeine Analysis in Health Functional Foods using HPLC-UVD (HPLC-UVD를 이용한 건강기능식품에서 클로로겐산과 카페인 동시분석법 최적화 및 적용성 검증)

  • Hee-Sun Jeong;Se-Yun Lee;Kyu-Heon Kim;Mi-Young Lee;Jung-Ho Choi;Jeong-Sun Ahn;Jae-Myoung Oh;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.61-71
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    • 2024
  • In this study, we analyzed chlorogenic acid indicator components in preparation for the additional listing of green coffee bean extract in the Health Functional Food Code and optimized caffeine for simultaneous analysis. We extracted chlorogenic acid and caffeine using 30% methanol, phosphoric acid solution, and acetonitrile-containing phosphoric acid and analyzed them at 330 and 280 nm, respectively, using liquid chromatography. Our analysis validation results yielded a correlation coefficient (R2) revealing a significance level of at least 0.999 within the linear quantitative range. The chlorogenic acid and caffeine detection and quantification limits were 0.5 and 0.2 ㎍/mL and 1.4, and 0.4 ㎍/mL, respectively. We confirmed that the precision and accuracy results were suitable using the AOAC validation guidelines. Finally, we developed a simultaneous chlorogenic acid and caffeine analysis approach. In addition, we confirmed that our analysis approach could simultaneously quantify chlorogenic acid and caffeine by examining the applicability of each formulation through prototypes and distribution products. In conclusion, the results of this study demonstrated that the standardized analysis would expectably increase chlorogenic acidcontaining health functional food quality control reliability.

Coupled T-H-M Processes Calculations in KENTEX Facility Used for Validation Test of a HLW Disposal System (고준위 방사성 폐기물 처분 시스템 실증 실험용 KENTEX 장치에서의 열-수리-역학 연동현상 해석)

  • Park Jeong-Hwa;Lee Jae-Owan;Kwon Sang-Ki;Cho Won-Jin
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.4 no.2
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    • pp.117-131
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    • 2006
  • A coupled T-H-M(Thermo-Hydro-Mechanical) analysis was carried out for KENTEX (KAERI Engineering-scale T-H-M Experiment for Engineered Barrier System), which is a facility for validating the coupled T-H-M behavior in the engineered barrier system of the Korean reference HLW(high-level waste) disposal system. The changes of temperature, water saturation, and stress were estimated based on the coupled T-H-M analysis, and the influence of the types of mechanical constitutive material laws was investigated by using elastic model, poroelastic model, and poroelastic-plastic model. The analysis was done using ABAQUS, which is a commercial finite element code for general purposes. From the analysis, it was observed that the temperature in the bentonite increased sharply for a couple of days after heating the heater and then slowly increased to a constant value. The temperatures at all locations were nearly at a steady state after about 37.5 days. In the steady state, the temperature was maintained at $90^{\circ}C$ at the interface between the heater and the bentonite and at about $70^{\circ}C$ at the interface between the bentonite and the confining cylinder. The variation of the water saturation with time in bentonite was almost same independent of the material laws used in the coupled T-H-M processes. By comparing the saturation change of T-H-M and that of H-M(Hydro-Mechanical) processes using elastic and poroelastic material mod31 respectively, it was found that the degree of saturation near the heater from T-H-M calculation was higher than that from the coupled H-M calculation mainly because of the thermal flux, which seemed to speed up the saturation. The stresses in three cases with different material laws were increased with time. By comparing the stress change in H-M calculation using poroelasetic and poroelasetic-plastic model, it was possible to conclude that the influence of saturation on the stress change is higher than the influence of temperature. It is, therefore, recommended to use a material law, which can model the elastic-plastic behavior of buffer, since the coupled T-H-M processes in buffer is affected by the variation of void ratio, thermal expansion, as well as swelling pressure.

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Preliminary Inspection Prediction Model to select the on-Site Inspected Foreign Food Facility using Multiple Correspondence Analysis (차원축소를 활용한 해외제조업체 대상 사전점검 예측 모형에 관한 연구)

  • Hae Jin Park;Jae Suk Choi;Sang Goo Cho
    • Journal of Intelligence and Information Systems
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    • v.29 no.1
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    • pp.121-142
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    • 2023
  • As the number and weight of imported food are steadily increasing, safety management of imported food to prevent food safety accidents is becoming more important. The Ministry of Food and Drug Safety conducts on-site inspections of foreign food facilities before customs clearance as well as import inspection at the customs clearance stage. However, a data-based safety management plan for imported food is needed due to time, cost, and limited resources. In this study, we tried to increase the efficiency of the on-site inspection by preparing a machine learning prediction model that pre-selects the companies that are expected to fail before the on-site inspection. Basic information of 303,272 foreign food facilities and processing businesses collected in the Integrated Food Safety Information Network and 1,689 cases of on-site inspection information data collected from 2019 to April 2022 were collected. After preprocessing the data of foreign food facilities, only the data subject to on-site inspection were extracted using the foreign food facility_code. As a result, it consisted of a total of 1,689 data and 103 variables. For 103 variables, variables that were '0' were removed based on the Theil-U index, and after reducing by applying Multiple Correspondence Analysis, 49 characteristic variables were finally derived. We build eight different models and perform hyperparameter tuning through 5-fold cross validation. Then, the performance of the generated models are evaluated. The research purpose of selecting companies subject to on-site inspection is to maximize the recall, which is the probability of judging nonconforming companies as nonconforming. As a result of applying various algorithms of machine learning, the Random Forest model with the highest Recall_macro, AUROC, Average PR, F1-score, and Balanced Accuracy was evaluated as the best model. Finally, we apply Kernal SHAP (SHapley Additive exPlanations) to present the selection reason for nonconforming facilities of individual instances, and discuss applicability to the on-site inspection facility selection system. Based on the results of this study, it is expected that it will contribute to the efficient operation of limited resources such as manpower and budget by establishing an imported food management system through a data-based scientific risk management model.

Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.