• Title/Summary/Keyword: Official Method

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Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

Intra-laboratory Validation of an HPLC Post-column Oxidation Method for the Analysis of PSP Toxins in Oysters and Mussels (굴과 진주담치 중 마비성 패류독소 분석을 위한 HPLC post-column oxidation method의 시험소 내 유효성 검증)

  • Song, Ki Cheol;Lee, Ka-Jeong;Yu, Hong-Sik;Mok, Jong-Soo;Kim, Ji Hoe;Lim, Keun-Sik;Lee, Mi-Ae;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.241-247
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    • 2013
  • AOAC Mouse Bioassay Analysis (MBA) has been the gold standard for the analysis of paralytic shellfish poisoning toxin (PSP toxin) for more than 50 years. However, this method has inaccurate limit of quantification and cannot be used to determine toxic profiles. An HPLC method (PCOX) was optimized for Korean shellfish to establish an alternative or supplementary method for PSP analysis and was intended to be used for the official monitoring and regulation of food. The recovery rate of the PCOX method was 83.5-112.1% and the limit of quantification for total toxin was about $8.6{\mu}g$/100 g. A long-term comparison study showed a good correlation of the PCOX results with the AOAC MBA results: the correlation factors were 0.9534 and 0.9109 for oyster and mussel matrices, respectively. The PCOX method may be used as an alternative or supplementary method for AOAC MBA to monitor the occurrence of PSP and to analyze PSP toxin profile in oysters and mussels.

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide- (식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-)

  • Chang, Hee-Ra;Kang, Hae-Rim;Kim, Jong-Hwan;Do, Jung-A;Oh, Jae-Ho;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.157-163
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    • 2012
  • BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

The Records and Archives Administrative Reform in China in 1930s (1930년대 중국 문서당안 행정개혁론의 이해)

  • Lee, Won-Kyu
    • The Korean Journal of Archival Studies
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    • no.10
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    • pp.276-322
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    • 2004
  • Historical interest in China in 1930s has been mostly focused on political characteristic of the National Government(國民政府) which was established by the KMT(中國國民黨) as a result of national unification. It is certain that China had a chance to construct a modern country by the establishment of the very unified revolutionary government. But, it was the time of expanding national crises that threatened the existence of the country such as the Manchurian Incident and the Chinese-Japanese War as well as the chaos of the domestic situation, too. So it has a good reason to examine the characteristic and pattern of the response of the political powers of those days. But, as shown in the recent studies, the manifestation method of political power by the revolutionary regime catches our attention through the understanding of internal operating system. Though this writing started from the fact that the Nationalist Government executed the administrative reform which aimed at "administrative efficiency" in the middle of 1930s, but it put stress on the seriousness of the problem and its solution rather than political background or results. "Committee on Administrative Efficiency(行政效率委員會)", the center of administrative reform movement which was established in 1934, examined the plan to execute the reform through legislation by the Executive Council(行政院) on the basis of the results of relevant studies. They claimed that the construction of a modern country should be performed by not political revolution anymore but by gradual improvement and daily reform, and that the operation of the government should become modern, scientific and efficient. There were many fields of administrative reform subjects, but especially, the field of records and archives adminstration(文書檔案行政) was studied intensively from the initial stage because that subject had already been discussed intensively. They recognized that records and archives were the basic tool of work performance and general activity but an inefficient field in spite of many input staff members, and most of all, archival reform bring about less conflicts than the fields of finance, organization and personnel. When it comes to the field of records adminstration, the key subjects that records should be written simply, the process of record treatment should be clear and the delay of that should be prevented were already presented in a records administrative meeting in 1922. That is, the unified law about record management was not established, so each government organization followed a conventional custom or performed independent improvement. It was through the other records administrative workshop of the Nationalist Government in 1933 when the new trend was appeared as the unified system improvement. They decided to unify the format of official records, to use marker and section, to unify the registration of receipt records and dispatch records and to strengthen the examination of records treatment. But, the method of records treatment was not unified yet, so the key point of records administrative reform was to establish a unified and standard record management system for preventing repetition by simplifying the treatment procedure and for intensive treatment by exclusive organizations. From the foundation of the Republic of China to 1930s, there was not big change in the field of archives administration, and archives management methods were prescribed differently even in the same section as well as same department. Therefore, the point at issue was to centralize scattered management systems that were performed in each section, to establish unified standard about filing and retention period allowance and to improve searching system through classification and proper number allowance. Especially, the problem was that each number system and classification system bring about different result due to dual operation of record registration and archives registration, and that strict management through mutual contrast, searching and application are impossible. Besides, various problems such as filing tools, arrangement method, preservation facilities & equipment, lending service and use method were raised also. In the process this study for the system improvement of records and archives management, they recognized that records and archives are the identical thing and reached to create a successive management method of records and archives called "Records and Archives Chain Management Method(文書檔案連鎖法)" as a potential alternative. Several principles that records and archives management should be performed unitedly in each organization by the general record recipient section and the general archives section under the principle of task centralization, a consistent classification system should be used by classification method decided in advance according to organizational constitution and work functions and an identical number system should be used in the process of record management stage and archive management stage by using a card-type register were established. Though, this "Records and Archives Chain Management Method" was developed to the stage of test application in several organizations, but it was not adopted as a regular system and discontinued. That was because the administrative reform of the Nationalist Government was discontinued by the outbreak of the Chinese-Japanese War. Even though the administrative reform in the middle of 1930s didn't produce practical results but merely an experimentation, it was verified that the reform against tradition and custom conducted by the Nationalist Government that aimed for the construction of a modern country was not only a field of politics, but on the other hand, the weak basis of the government operation became the obstacle to the realization of the political power of the revolutionary regime. Though the subject of records and archives administrative reform was postponed to the future, it should be understood that the consciousness of modern records and archives administration and overall studies began through this examination of administrative reform.

Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 Spinetoram 공정시험법 개발 및 검증)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun Hyang;Ju, Yun Ji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.94-103
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    • 2016
  • An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.

Comparison Study on Efficacies of Disinfectants and Sanitizers Among Methods for Quantitative Surface Test (살균소독제의 정량적 표면시험방법별 유효성 비교)

  • Kim, Ae-Young;Kim, Yong-Su;Ha, Sang-Do
    • Journal of Food Hygiene and Safety
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    • v.25 no.3
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    • pp.238-244
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    • 2010
  • Currently, in vitro suspension tests using tubes are used as a authorized test method for sanitizers and disinfectants. However, the methods could not accurately assess the efficacy of sanitizers and disinfectant on the food-contacted surfaces in the field. This study evaluated the effectiveness of 5 kinds of representative sanitizers and disinfectants against E. coli and S. aureus to compare three quantitative surface testing methods that have been internationally standardized. As a result, the ASTM E2111-05 (ASTM(1)) test method obtained 5.18 $\pm$ 0.03 and 5.27 $\pm$ 0.04 log cfu/carrier reduction in dealing with E. coli and S. aureus, respectively, the ASTM E2197-02 (ASTM(2)) test method obtained 4.63 $\pm$ 0.04 and 3.97 $\pm$ 0.03 log cfu/carrier reduction and the CEN EN 13697 test method should 6.14 $\pm$ 0.05 and 5.31 $\pm$ 0.10 log cfu/carrier reduction in clean condition (CEN(1)) but 4.37 $\pm$ 0.02 and 4.06 $\pm$ 0.01 log cfu/carrier reduction in dirty condition (CEN(2)). Among them, CEN(1) showed the highest bactericidal effects, whereas ASTM(2) and CEN(2) revealed low performance (p < 0.05). In conclusion, the bactericidal effects of the ASTM(2) method and the CEN EN 13697 method adopting stainless steel were lower than the ASTM(1) method, which uses glass. The effectiveness assessment results among nationally accredited test methods were different each other. This implies that they could not fit for in the accurate evaluation of sanitization and disinfection on food-contact surfaces in practical food-processing fields. These results could be used as a basic data for establishment of an official surface test methods applicable in the field.

Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

Availability of Heavy Metals in Soils with Different Characteristics and Controversial Points for Analytical Methods of Soil Contamination in Korea (토양특성별 중금속 유효도와 토양오염 평가방법의 개선점)

  • Jung, Goo-Bok;Kim, Won-Il;Lee, Jong-Sik;Shin, Joung-Du;Kim, Jin-Ho;Yun, Sun-Gang
    • Korean Journal of Environmental Agriculture
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    • v.24 no.2
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    • pp.106-116
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    • 2005
  • This experiment was conducted to investigate available extraction capacity and potential mobility of heavy metal according to the distribution property and contamination level of heavy metals in soils and to suggest a reform measure of soil environment assessment methodology applied with soil quality and the official soil heavy metal test methods in domestic and foreign countries. The soils were collected from the natural forest paddy with long-term application of same type fertilizer, and paddies near metal mine and industrial complex. The post-treatment methods of soil were partial extraction, acid digestion and sequential extraction methods. For the heavy metal contents with different soil properties, it was shown that their natural forest and paddy soil were slightly low and similar to the general paddy soil, while their paddies near metal mine and industrial complex were higher than the standard level of Soil Environment Protection Act. Heavy metal concentrations in the soils with different soil properties had difference between $HNO_3\;and\;HNO_3+HCl$ extractant by US-EPA 3051a method. There were highly significant positive relationships in both two methods. It was appeared that the higher extractable concentration ratio with 0.1N-HCl to total heavy metal content with $HNO_3+HCl$ extractant the greater total heavy metal content. There were highly significant positive correlationship between total heavy metal content and extractable content with 0.1N-HCl. For extractable capacity of soil extractable solution compared to the total heavy metal content it was appeared that it extractable method with 0.1N-HCl was higher than those with EDTA and DTPA. In extractable ratio with 0.1N-HCl in the contaminated paddy soils near mine and industrial complex, it was shown that the lower soil pH, the higher total heavy metal content. The order of a potential mobility coefficient by distribution of heavy metal content with ie different typies in the soil was Cd>Ni>Zn>Cu>Pb. It could be known that contamination characteristics of heavy metals with different types of soils were affected by different heavy metal components, contamination degree and soil chemical properties, and heavy metal concentration with different extractable methods had great variations with adjacent environment. To be compared with assessment methodology of soil environment impact at domestic and foreign countries with our results, it might be considered that there was necessary to make a single analysis method based on total heavy metal content with environmental overloading concept because of various analysis methods for total heavy metal content and present analysis method with great variation according to soil environment. In spite of showing higher concentration of heavy metal with acidic digestion than the extractable method, it might be considered that there is need to be adjusted the national standard of soil heavy metal contamination.

Development of Analysis Method for Cholesterol in Infant Formula by Direct Saponification (직접 검화법을 이용한 조제분유의 콜레스테롤 분석법 개발)

  • Kim, Jin-Man;Park, Jung-Min;Yoon, Tae-Hyung;Leem, Dong-Gil;Yoon, Chang-Yong;Jeong, Ja-Young;Jeong, In-Seek;Kwak, Byung-Man;Ahn, Jang-Hyuk
    • Food Science of Animal Resources
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    • v.31 no.6
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    • pp.944-951
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    • 2011
  • An improved cholesterol analysis method was developed for powdered infant formula by gas chromatographic separation after liquid-liquid extraction and partition. In the official Korea Food Standard method for cholesterol analysis, the water phase and solvent phase were not well separated in the case of emulsified foods such as powdered infant formulas and baby foods. For the rapid and simple sample preparation method, an optimized direct saponification condition was established for heating temperature, heating time, and KOH concentration. From the results, the optimum conditions were as follows: heating temperature $90^{\circ}C$, heating time 60 min, and 16 M KOH 10 mL for a 2 g infant formula sample; improved separation condition for gas chromatography was as follows: the initial oven condition was $250^{\circ}C$ for 25 min, the oven temperature was increased to $290^{\circ}C$ by $10^{\circ}C$/min ratio, and finally the oven temperature remained at $290^{\circ}C$for 9 min. The developed method could be implemented for the study of cholesterol, providing the advantages of reduced inspection time and cost in emulsified foods such as infant formula.

Development and Validation of an Analytical Method for Determination of Fungicide Benzovindiflupyr in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 벤조빈디플루피르의 잔류시험법 개발 및 검증)

  • Lim, Seung-Hee;Do, Jung-Ah;Park, Shin-Min;Pak, Won-Min;Yoon, Ji Hye;Kim, Ji Young;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.298-305
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    • 2017
  • Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.