• Title/Summary/Keyword: Advanced monitoring

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Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

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.

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.

Regulatory Mechanism of Insulin-Like Growth Factor Binding Protein-3 in Non-Small Cell Lung Cancer (비소세포성 폐암에서 인슐린 양 성장 인자 결합 단백질-3의 발현 조절 기전)

  • Chang, Yoon Soo;Lee, Ho-Young;Kim, Young Sam;Kim, Hyung Jung;Chang, Joon;Ahn, Chul Min;Kim, Sung Kyu;Kim, Se Kyu
    • Tuberculosis and Respiratory Diseases
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    • v.56 no.5
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    • pp.465-484
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    • 2004
  • Background : Insulin-like growth factor (IGF)-binding protein-3 (IGFBP-3) inhibits the proliferation of non-small cell lung cancer (NSCLC) cells by inducing apoptosis. Methods : In this study, we investigated whether hypermethylation of IGFBP-3 promoter play an important role in the loss of IGFBP-3 expression in NSCLC. We also studied the mechanisms that mediate the silencing of IGFBP-3 expression in the cell lines which have hypermethylated IGFBP-3 promoter. Results : The IGFBP-3 promoter has hypermethylation in 7 of 15 (46.7%) NSCLC cell lines and 16 (69.7%) of 23, 7 (77.8%) of 9, 4 (80%) of 5, 4 (66.7 %) of 6, and 6 (100%) of 6 tumor specimens from patients with stage I, II, IIIA, IIIB, and IV NSCLC, respectively. The methylation status correlated with the level of protein and mRNA in NSCLC cell lines. Expression of IGFBP-3 was restored by the demethylating agent 5'-aza-2'-deoxycytidine (5'-aza-dC) in a subset of NSCLC cell lines. The Sp-1/ Sp-3 binding element in the IGFBP-3 promoter, important for promoter activity, was methylated in the NSCLC cell lines which have reduced IGFBP-3 expression and the methylation of this element suppressed the binding of the Sp-1 transcription factor. A ChIP assay showed that the methylation status of the IGFBP-3 promoter influenced the binding of Sp-1, methyl-CpG binding protein-2 (MeCP2), and histone deacetylase (HDAC) to Sp-1/Sp-3 binding element, which were reversed by by 5'-aza-dC. In vitro methylation of the IGFBP-3 promoter containing the Sp-1/Sp-3 binding element significantly reduced promoter activity, which was further suppressed by the overexpression of MeCP2. This reduction in activity was rescued by 5'-aza-dC. Conclusion : These findings indicate that hypermethylation of the IGFBP-3 promoter is one mechanism by which IGFBP-3 expression is silenced and MeCP2, with recruitment of HDAC, may play a role in silencing of IGFBP-3 expression. The frequency of this abnormality is also associated with advanced stages among the patients with NSCLC, suggesting that IGFBP-3 plays an important role in lung carcinogenesis/progression and that the promoter methylation status of IGFBP-3 may be a marker for early molecular detection and/or for monitoring chemoprevention efforts.

A New Exploratory Research on Franchisor's Provision of Exclusive Territories (가맹본부의 배타적 영업지역보호에 대한 탐색적 연구)

  • Lim, Young-Kyun;Lee, Su-Dong;Kim, Ju-Young
    • Journal of Distribution Research
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    • v.17 no.1
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    • pp.37-63
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    • 2012
  • In franchise business, exclusive sales territory (sometimes EST in table) protection is a very important issue from an economic, social and political point of view. It affects the growth and survival of both franchisor and franchisee and often raises issues of social and political conflicts. When franchisee is not familiar with related laws and regulations, franchisor has high chance to utilize it. Exclusive sales territory protection by the manufacturer and distributors (wholesalers or retailers) means sales area restriction by which only certain distributors have right to sell products or services. The distributor, who has been granted exclusive sales territories, can protect its own territory, whereas he may be prohibited from entering in other regions. Even though exclusive sales territory is a quite critical problem in franchise business, there is not much rigorous research about the reason, results, evaluation, and future direction based on empirical data. This paper tries to address this problem not only from logical and nomological validity, but from empirical validation. While we purse an empirical analysis, we take into account the difficulties of real data collection and statistical analysis techniques. We use a set of disclosure document data collected by Korea Fair Trade Commission, instead of conventional survey method which is usually criticized for its measurement error. Existing theories about exclusive sales territory can be summarized into two groups as shown in the table below. The first one is about the effectiveness of exclusive sales territory from both franchisor and franchisee point of view. In fact, output of exclusive sales territory can be positive for franchisors but negative for franchisees. Also, it can be positive in terms of sales but negative in terms of profit. Therefore, variables and viewpoints should be set properly. The other one is about the motive or reason why exclusive sales territory is protected. The reasons can be classified into four groups - industry characteristics, franchise systems characteristics, capability to maintain exclusive sales territory, and strategic decision. Within four groups of reasons, there are more specific variables and theories as below. Based on these theories, we develop nine hypotheses which are briefly shown in the last table below with the results. In order to validate the hypothesis, data is collected from government (FTC) homepage which is open source. The sample consists of 1,896 franchisors and it contains about three year operation data, from 2006 to 2008. Within the samples, 627 have exclusive sales territory protection policy and the one with exclusive sales territory policy is not evenly distributed over 19 representative industries. Additional data are also collected from another government agency homepage, like Statistics Korea. Also, we combine data from various secondary sources to create meaningful variables as shown in the table below. All variables are dichotomized by mean or median split if they are not inherently dichotomized by its definition, since each hypothesis is composed by multiple variables and there is no solid statistical technique to incorporate all these conditions to test the hypotheses. This paper uses a simple chi-square test because hypotheses and theories are built upon quite specific conditions such as industry type, economic condition, company history and various strategic purposes. It is almost impossible to find all those samples to satisfy them and it can't be manipulated in experimental settings. However, more advanced statistical techniques are very good on clean data without exogenous variables, but not good with real complex data. The chi-square test is applied in a way that samples are grouped into four with two criteria, whether they use exclusive sales territory protection or not, and whether they satisfy conditions of each hypothesis. So the proportion of sample franchisors which satisfy conditions and protect exclusive sales territory, does significantly exceed the proportion of samples that satisfy condition and do not protect. In fact, chi-square test is equivalent with the Poisson regression which allows more flexible application. As results, only three hypotheses are accepted. When attitude toward the risk is high so loyalty fee is determined according to sales performance, EST protection makes poor results as expected. And when franchisor protects EST in order to recruit franchisee easily, EST protection makes better results. Also, when EST protection is to improve the efficiency of franchise system as a whole, it shows better performances. High efficiency is achieved as EST prohibits the free riding of franchisee who exploits other's marketing efforts, and it encourages proper investments and distributes franchisee into multiple regions evenly. Other hypotheses are not supported in the results of significance testing. Exclusive sales territory should be protected from proper motives and administered for mutual benefits. Legal restrictions driven by the government agency like FTC could be misused and cause mis-understandings. So there need more careful monitoring on real practices and more rigorous studies by both academicians and practitioners.

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A Study on the Application of Outlier Analysis for Fraud Detection: Focused on Transactions of Auction Exception Agricultural Products (부정 탐지를 위한 이상치 분석 활용방안 연구 : 농수산 상장예외품목 거래를 대상으로)

  • Kim, Dongsung;Kim, Kitae;Kim, Jongwoo;Park, Steve
    • Journal of Intelligence and Information Systems
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    • v.20 no.3
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    • pp.93-108
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    • 2014
  • To support business decision making, interests and efforts to analyze and use transaction data in different perspectives are increasing. Such efforts are not only limited to customer management or marketing, but also used for monitoring and detecting fraud transactions. Fraud transactions are evolving into various patterns by taking advantage of information technology. To reflect the evolution of fraud transactions, there are many efforts on fraud detection methods and advanced application systems in order to improve the accuracy and ease of fraud detection. As a case of fraud detection, this study aims to provide effective fraud detection methods for auction exception agricultural products in the largest Korean agricultural wholesale market. Auction exception products policy exists to complement auction-based trades in agricultural wholesale market. That is, most trades on agricultural products are performed by auction; however, specific products are assigned as auction exception products when total volumes of products are relatively small, the number of wholesalers is small, or there are difficulties for wholesalers to purchase the products. However, auction exception products policy makes several problems on fairness and transparency of transaction, which requires help of fraud detection. In this study, to generate fraud detection rules, real huge agricultural products trade transaction data from 2008 to 2010 in the market are analyzed, which increase more than 1 million transactions and 1 billion US dollar in transaction volume. Agricultural transaction data has unique characteristics such as frequent changes in supply volumes and turbulent time-dependent changes in price. Since this was the first trial to identify fraud transactions in this domain, there was no training data set for supervised learning. So, fraud detection rules are generated using outlier detection approach. We assume that outlier transactions have more possibility of fraud transactions than normal transactions. The outlier transactions are identified to compare daily average unit price, weekly average unit price, and quarterly average unit price of product items. Also quarterly averages unit price of product items of the specific wholesalers are used to identify outlier transactions. The reliability of generated fraud detection rules are confirmed by domain experts. To determine whether a transaction is fraudulent or not, normal distribution and normalized Z-value concept are applied. That is, a unit price of a transaction is transformed to Z-value to calculate the occurrence probability when we approximate the distribution of unit prices to normal distribution. The modified Z-value of the unit price in the transaction is used rather than using the original Z-value of it. The reason is that in the case of auction exception agricultural products, Z-values are influenced by outlier fraud transactions themselves because the number of wholesalers is small. The modified Z-values are called Self-Eliminated Z-scores because they are calculated excluding the unit price of the specific transaction which is subject to check whether it is fraud transaction or not. To show the usefulness of the proposed approach, a prototype of fraud transaction detection system is developed using Delphi. The system consists of five main menus and related submenus. First functionalities of the system is to import transaction databases. Next important functions are to set up fraud detection parameters. By changing fraud detection parameters, system users can control the number of potential fraud transactions. Execution functions provide fraud detection results which are found based on fraud detection parameters. The potential fraud transactions can be viewed on screen or exported as files. The study is an initial trial to identify fraud transactions in Auction Exception Agricultural Products. There are still many remained research topics of the issue. First, the scope of analysis data was limited due to the availability of data. It is necessary to include more data on transactions, wholesalers, and producers to detect fraud transactions more accurately. Next, we need to extend the scope of fraud transaction detection to fishery products. Also there are many possibilities to apply different data mining techniques for fraud detection. For example, time series approach is a potential technique to apply the problem. Even though outlier transactions are detected based on unit prices of transactions, however it is possible to derive fraud detection rules based on transaction volumes.