• Analytical Science and Technology
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• 제23권3호
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• pp.247-254
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• 2010

This study was carried out to produce Reference Materials (RMs) for Proficiency Testing (PT) of PCBs in waste analytical laboratories. Two RMs were prepared from used transformer oil samples and PCB free transformer oil by spiking PCBs standard solutions. The spiked PCB RMs were homogenized by mixing and settling up to 90 days. Homogenized concentration of PCBs with Arochlor 1254 (6 ppm), 1254:1260 (1:1) (5 ppm) were observed in 60 days stationary phase but Arochlor 1260 (3.5 mg/L) were observed in 90 days stationary phase. One-way ANOVA test were carried out and showed that the RMs were suitably homogenized, which can be used for proficiency testing. The Relative Standard Deviations (RSDs) of analytical results were 3.51~5.01% for the PCBs RMs in 10 replicates. The expanded uncertainty of PCBs analytical procedure were 0.26~0.49.

• Clinical and Experimental Pediatrics
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• 제50권2호
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• pp.143-150
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• 2007

Purpose : This study was conducted to validate enzyme immunoassay (EIA) for the quantitative measurement of human IgG antibodies specific for Haemophilus influenzae type b (Hib) capsular polysaccharide. Method : We evaluated specificity, repeatability, intermediate precision, accuracy, lower limit of quantification (LLOQ), and stability to validate standardized EIA for the quantitative measurement of human anti-polyribosylribitol phosphate (PRP) IgG antibodies. Results : The results indicated that this EIA showed specificity to HbO-HA antigen and repeatability and intermediate precision were within acceptance criteria (repeatability: $CV{\leq}15%$, intermediate precision: $CV{\leq}20%$). The EIA-derived results from this laboratory were equivalent to those obtained by the standard radioactive antigen binding assay (RABA) for quantitation of anti-PRP antibodies in the 28 sera. Spiking recovery result was within acceptance criteria ($100{\pm}20%$). The precision and accuracy of samples in LLOQ were from -14.7 to -4.7% in nominal values, which were within acceptance criteria (precision: $CV{\leq}25%$, accuracy: ${\pm}25%$). Freeze-thaw stability and short term temperature stability were within ${\pm}20%$ of acceptance criteria. Conclusions : The EIA which is performed at the Center for Vaccine Evaluation and Study Ewha Medical Research Institute, is an appropriate serologic assay which can be used for quantitation of anti-PRP IgG antibodies in human sera.

• Journal of Korean Society on Water Environment
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• 제22권2호
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• pp.321-327
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• 2006

This interlaboratory study was designed to evaluate protozoan test methods in water and to predict the major causes of deviation of the methods. Each of four laboratories with previous experience of protozoa analysis in water participated, and met the initial performance criteria of EPA 1623 method provided. The protozoan analysis procedure consists of filtrations, concentration, immunomagnetic separation, dyeing (staining) and counting with observation. We tested three different filtration equipments: capsule filter for 10 L of surface water, and high volume (HV) capsule filter and membrane filter for 100 L of finished water. When the recovery of each step of the procedure was evaluated with EasySeed, the commercial stock of each 100 Cryptosporidium and Giardia, immunomagnetic separation and filtration step were the most crucial steps affecting the stability of the recovery, especially for Cryptosporidium. There was no significant difference of recovery among the filtration methods. Recovery of protozoa from source water were evaluated with spiked EasySeed as matrix tests. The recoveries of Giardia increased significantly in the matrix tests compared those in the deionized water. We also applied red stained mixture stocks of Cryptosporidium and Giardia called ColorSeed as internal standards of water sample tests. The recoveries of both EasySeed and ColorSeed in samples tested were within the range of the criteria, however, the Giardia recoveries using ColorSeed decreased significantly. Further optimization study with ColorSeed will be necessary, considering the convenience of using the internal standard without additional sample analysis. The significant factors of the recovery variation were identified as the differences of laboratories as well as water quality and type of the stock for spiking. The results of this study emphasize the importance of the quality assurance program for protozoan analysis lab in water.

• Journal of Food Hygiene and Safety
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• 제23권4호
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• pp.319-323
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• 2008

Analytical method for determination of florfenicol was developed for estimate veterinary drug residue of unestablished MRLs in meat. The method was validated in correspondence with the CODEX guideline for florfenicol residue in meat. The samples mixed with sodium sulfate were extracted with ethyl acetate. After clean-up, the residue was dissolved in mobile phase and analyzed using high-performance liquid chromatography with fluorescence detector. The calibration curve showed good linearity($r^2=0.9997$) within the concentration range of $0.05{\sim}1.0\;mg/kg$. The limit of detection(LOD) and limit of quantification(LOQ) were validated at 0.012 and 0.039 mg/kg, respectively. The recoveries in fortified meat ranged from 85.6 to 95.6%($1.1{\sim}5.3%$ RSD) at the 0.05 to 0.4 spiking levels. We monitored 150 samples of meats that were purchased in Korea(Seoul, Busan, Daegu, Daejeon and Gwangju). Among tested samples, florfenicol was detected in 1 of pig at the level of 0.040 mg/kg, and below LOQ in 1 of cattle, 2 of pig and 2 of chicken. The residues of florfenicol in the tested samples were within the MRLs.

• Journal of Food Hygiene and Safety
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• 제25권3호
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• pp.226-231
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• 2010

We aimed at the monitoring medroxyprogesterone acetate (MPA) residue amount in meats and confirmed the safety of its residue in meats. Optimized condition for analytical and instrumental methods was obtained by method validation. The limit of detection (LOD) and limit of quantification (LOQ) were validated at 1.5 and 5.0 ug/kg, respectively. The calibration curve showed good linearity ($r^2$ = 0.9968) within the concentration range of 5.0~50.0 ug/kg. We selected progesterone-d9 for internal standard, The recoveries in fortified meat ranged from 67.5 to 109.56% at the 3 spiking levels. As the regulation of MPA analysis method used by LC-MS/MS on other products have established. We selected 3 species of farm stock products (cattle, pig, chicken) and purchased at the markets of seven major cities. The total 196 of meat including 46 of domestic beef, 43 of import beef, 60 of domestic pork, 12 of import pork and 35 of domestic chicken. No residue of synthetic growth hormones were detected in cattle, pig and chicken samples tested.

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
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• 한국축산식품학회 2005년도 정기총회 및 제35차 춘계 학술 발표대회
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• pp.231-234
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• 2005

본 실험은 돈육 후지 부위를 이용하여 육포 제조시 텀블링 시간에 따른 육포의, 이화학적 및 관능적 특성을 조사하여 표준화된 육포제조의 기초 자료를 제공하고자 실시하였다. 텀블링 시간에 따른 건조전 육포 양념육의 제품수율은 30분까지는 수율이 유의적으로 증가하는 경향을 보였으나, 60분 동안 텀블링을 실시하였을 때는 30분보다 낮은 값을 나타내었다. 텀블링 시간에 따라 pH는 차이가 없었으나, 보수력은 텀블링 30분까지 유의적으로 증가하였고 이후 부터는 차이가 없었다. 육색은 텀블링 시간이 경과함에 따라 $L^{\ast}-$값과 $b^{\ast}-$값은 감소하는 경향을 보였으나 반대로 $a^{\ast}-$값은 텀블링 시간이 증가함에 따라 점점 증가하는 경향을 보였다. 건조후 제조된 돈육육포의 수분함량은 $29{\sim}30%$ 정도를 유지하였으며, 건조수율은 모두 $48{\sim}49%$ 정도의 높은 수율을 보였다. 육포의 $L^{\ast}-$값은 30분 및 60분 동안 텀블링을 실시하였을 때 10분 동안 텀블링을 실시한 육포보다 낮게 나타났다. 60분 동안 텀블링한 육포의 $a^{\ast}-$값은 10분간 텀블링한 것보다 높았으며, $b^{\ast}-$값은 $a^{\ast}-$값과는 반대의 경향을 나타내었다. 탄력성(springiness)은 60분 동안 텀블링한 육포가 10분 동안 텀블링한 육포보다 높은 값을 보였으나, 탄력성을 제외한 모든 항목에서 유의차가 나타나지 않았다. 관능검사는 모든 항목에서 30분 이상 텀블링한 육포가 좋은 평가를 받았으나, 처리구간에 유의차는 나타나지 않았다.pm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.화와 네트워크 조직망 구축을 위한 지역중심의 복합 생활문화 공간이 필요할 것이며, 이를 촉진키 위한 mentor academy시스템 접근을 통해 점점 고령화되어 가고 있는 재래시장에 대해 차별적 특성이 반영된 종합적이고 체계적 접근 방법연구가 필요하다./TEX> 자체기술개발, 선진기술 도입, 산업간 및 산업내 기술확산, 국제기술협력 ${\rightarrow}$ 기술혁신의 촉진 ${\rightarrow}$ 총요소생산성과 기업경쟁력(자원 및 역량, 프로세스 경쟁력, 품질경쟁력, 시장경쟁력, 고객성과, 시장성과, 재무성과)의 제고 ${\rightarrow}$ 가격경쟁력(임금, 금리, 물류비용, 환율 등)과 비(非)가격경쟁력(디자인, 에프터서비스, 품질, 운송 등)의 제고 ${\rightarrow}$ 국가경쟁력의 제고 ${\rightarrow}$ 국제수지 흑자 ${\ri

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
• /
• 한국축산식품학회 2005년도 정기총회 및 제35차 춘계 학술 발표대회
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• pp.247-252
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• 2005

본 연구는 파슬리 등의 야채를 첨가하여 제조되는 화이트소시지의 물성 및 저장성에 미치는 자두 분말의 효과를 조사하기 위해 실시되었다. 물성의 변화로서 pH는 자두의 첨가율이 증가함에 따라 상대적으로 감소 하였는데 3% 첨 가시 전 저장 기간 중 가장 낮게 ($pH\;5.11\;{\sim}\;4.44$) 나타났다. 육색(meat color)은 자두의 첨가량에 비례하여 적색도(redness)를 나타내는 a-value에서 높게 나타났으며 명도 (light ness)를 나타내는 L-value에서는 상대적으로 낮은 수치를 보여주었다. 전단력(Shear stre ngth) 측정에서는 저장 기간 중 자두 분말의 첨가량에 비례 하여 근소한 차이를 나타냈는데 저장 7일째에서 가장 높았다. 자두 분말 첨가구 에서의 다소 높은 전단력의 결과는 보수력 (WHC) 측정 에서도 같은 경향을 나타내었는데 자두 분말의 증가량에 따라 3% 첨가구가 대조구 (0%)보다 낮게 나타나 약한 보수성을 보여 주었다. 저장성에 미치는 결과로서 총세균수의 측정결과 저장 3일이 경과한 구간에서 Sorbic acid (0.07%)의 첨가구와 자두 분말(3%) 첨가구 에서 비슷한 항균 효과를 나타내었다. 이 같은 동일한 수준의 항균 효과는 저장 9일째에도 같은 경향으로 나타났다. VBN 측정에는 저장 기간에 따라 증가된 수치를 나타냈는데 저장 7일 및 8일, 9일째 측정 결과는 3% 자두분말 첨가구와 0.07% Sorbic acid 첨가구 와 비슷한 수준을 나타내어 동일한 저장효과를 보여 주었다. 관능검사 실시 결과 총체적인 풍미에 있어서는 자두 분말 첨가구 1.5%가 가장 우수 했으며 다음으로는 3%, Sorbic acid 첨가구 및 공시료 순으로 나타났다.간에 유의차는 나타나지 않았다.pm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.화와 네트워크 조직망 구축을 위한 지역중심의 복합 생활문화 공간이 필요할 것이며, 이를 촉진키 위한 mentor academy시스템 접근을 통해 점점 고령화되어 가고 있는 재래시장에 대해 차별적 특성이 반영된 종합적이고 체계적 접근 방법연구가 필요하다./TEX> 자체기술개발, 선진기술 도입, 산업간 및 산업내 기술확산, 국제기술협력 ${\rightarrow}$ 기술혁신의 촉진 ${\rightarrow}$ 총요소생산성과 기업경쟁력(자원 및 역량, 프로세스 경쟁력, 품질경쟁력, 시장경쟁력, 고객성과, 시장성과, 재무성과)의 제고 ${\rightarrow}$ 가격경쟁력(임금, 금리, 물류비용, 환율 등)과 비(非)가격경쟁력(디자인, 에프터서비스, 품질, 운송 등)의 제고 ${\rightarrow}$ 국가경쟁력의 제고 ${\rig

• Korean Journal of Environmental Agriculture
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• 제39권3호
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• Korean Journal of Food Science and Technology
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• 제45권4호
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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 ($R^2$ >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.

• Analytical Science and Technology
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• 제30권5호
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• pp.295-302
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• 2017

This study presents a method validation for extraction and quantitative analysis of levulinic acid in soy sacues using high performance liquid chromatograph-photodiode array detector (HPLC-PDA). The levulinic acid in samples were extracted with distilled water, and then purified with C18 Sep-Pak cartridge. The calibration curves showed good linearity (R > 0.999) in a relatively wide concentration range ($2.5-400{\mu}g/mL$). Mean recoveries and relative standard deviation (RSD) of levulinic acid spiked in soy sauce samples at different spiking levels ($2.5-400{\mu}g/mL$; 6 point). Recoveries were 87.58-97.26 % with RSD less than 15 %, and limit of detection (LOD) and limit of quantification (LOQ) were 0.64 and $1.64{\mu}g/mL$, respectively. According to monitoring result with the established method, levulinic acid was found in 43 of 59 domestic commercial soy sauces, soy sauce based sauces and seasoned meats. The contamination levels were 0.44-1.23 mg/mL for soy sauces, 0.03-0.83 mg/mL for soy sauce based sauces and 8.43-38.94 mg/mL for seasoned meats. The results indicated to be rapidly and accurately qualifying levulinic acid and can be used as a suitable quality control method for soy sauce and soy sauce related commodities.