• Journal of Food Hygiene and Safety
• /
• v.27 no.4
• /
• pp.332-338
• /
• 2012

A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

• Journal of Applied Biological Chemistry
• /
• v.64 no.2
• /
• pp.177-184
• /
• 2021

While veterinary antibiotics are used only in a part of the dose administered, the rest are excreted as urine or feces. Residual antibiotics enter the adjacent agricultural environments by spraying manure-based composts on farmlands and lead to secondary pollution. Therefore, it is necessary to develop the technique for post management such as regulatory levels of antibiotics in the agricultural environments. This study was conducted to compare by different matrices the amount of residual antibiotics such as tetracyclines and sulfonamides, which are known to be frequently used in Korea and to practice risk assessment by different antibiotics in soils before and after application of composts. Pre-treatment with modified typical method using buffer and solid phase extraction showed the recovery of composts and soils was more than 70% at ppb level and the limits of detection were 0.13-0.46 and 0.05-0.25 ㎍/kg, respectively. Analysis of manure-based composts revealed concentrations from 5.38 to 196.0 ㎍/kg for tetracyclines, from below the detection of limit (BDL) to 259.0 ㎍/kg for sulfonamides. In case of agricultural soils, residual concentrations of selected veterinary antibiotics were ranged 0.30-53.3 ㎍/kg, BDL-4.16 ㎍/kg respectively and the concentration level of tetracyclines, which had higher soil distribution coefficient (Kd) values, was higher than that of sulfonamides. There was a difference in human risk assessment by different antibiotics in soil before and after application of composts. But, it was indicated that detection values of all of 5 antibiotics were very safe on the basis that Hazard Quotient was safe below 1.

• Analytical Science and Technology
• /
• v.20 no.5
• /
• pp.424-433
• /
• 2007

An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

• Analytical Science and Technology
• /
• v.21 no.3
• /
• pp.183-190
• /
• 2008

PFOS (Perfluorooctane sulfonate) and PFOA (Perfluorooctanoic acid) are environmental hormones which belong to potential future persistent organic pollutants (POPs), and it is easy to exposure to human because they are used in a wide variety of consumer products. We studied exposure route and the relativity through determining and monitoring of PFOS and PFOA in Korean plasma of metropolis, small town, rural area and industrial area. And we monitored the concentration of PFOS and PFOA regarding the gender and age. The older age is, the higher concentration of PFOS is. The mean concentration of PFOS and PFOA in men (4.74 ng/mL, 2.20 ng/mL) was higher than that in women (3.53 ng/mL, 1.17 ng/mL). In the comparison of residential areas, the mean concentration of PFOS and PFOA was the lowest in metropolitan plasma (2.47 ng/mL, 0.79 ng/mL) whereas it was the highest in the industrial area (6.57 ng/mL, 2.19 ng/mL).

• Analytical Science and Technology
• /
• v.21 no.4
• /
• pp.259-271
• /
• 2008

The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with $85{\mu}m$, adsorption time was for 5 min, adsorption optimum temperature was at $280^{\circ}C$, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs.

• Journal of Applied Biological Chemistry
• /
• v.66
• /
• pp.258-265
• /
• 2023

After application of veterinary antibiotics, they may be partially metabolized before they are excreted by feces or urine either as unaltered form or as metabolites. Residual antibiotics enter the adjacent agricultural environments by spraying manure-based compost and liquid fertilizer on farmlands and lead to secondary pollution. The objective of this study was to compare the residual concentrations of 6 veterinary antibiotics by different production stages of liquid fertilizer from livestock manure recycling facilities. The relationship between concentration change of the residual antibiotics and the amount of liquid fertilizer component was also assessed. Pre-treatment showed the recovery of 63.4-106.7% at ppb level and the limit of quantification of 0.009-0.037 ㎍/L.As the result of analyzing the relationship between the residual concentrations of antibiotics and the amount of N component in liquid fertilizer by different production stages, the residual concentrations of antibiotics and N tended to decrease as the stabilization period elapsed during the liquid fertilization process. Average concentrations of sulfamethazine in raw materials, middle and final products of liquid fertilizer were 40.85, 26.17, 3.54 ㎍/L, respectively. Those of chlortetracycline decreased from 2.32 to 1.25 ㎍/L. The other 4 antibiotics also showed a decreasing trend by different production stages of liquid fertilizer. The amount of liquid fertilizer component N decreased from 0.21 to 0.096% by production stages of liquid fertilizer. It is considered that the correlation between residual antibiotic concentrations and N content can be applied as basic data for setting antibiotic reduction indicators.

• Journal of Food Hygiene and Safety
• /
• v.31 no.5
• /
• pp.319-326
• /
• 2016

Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
• /
• 2005.05a
• /
• pp.247-252
• /
• 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

• YAKHAK HOEJI
• /
• v.52 no.2
• /
• pp.137-146
• /
• 2008

Even though driving under the influence of drug (DUID) is a worldwide problem, we, Korea has no regulation system yet except for alcohol, and there are little cases reported related to DUID. In order to investigate the type of abused drugs for drivers in Korea, we tried to analyze controlled and non-controlled drugs in alcohol-positive blood samples. 275 whole bloods, which were positive for alcohol on the roadside test, were collected from the police for two months ($Nov.{\sim}Dec.$ 2006). The analytical strategy was constituted of three steps: First, alcohol in blood samples were confirmed and quantified by gas chromatography. Second, controlled drugs were screened by $Evidence_{investigator}\;^{TM}$ (Randox, U.K.) as preliminary test. It was based on immunoassay by biochip array analyzer. Nine groups of drug abuse were screened: amphetamines, methamphetamines, cannabis, cocaine, opiates, barbiturates, methadone, benzodiazepines I (oxazepam) & II (lorazepam). Finally, confirmation of these drugs was performed by GC-MS. Blood samples were extracted by solid-phase extraction by $RapidTrace^{TM}$ (Zymark, U.S.A.). After trimethylsilyl (TMS) derivatization, eluates were analyzed to GC-MS. Total 49 drugs were investigated in this study including controlled drugs, antidepressants, 1st generation antihistamines, dextromethorphan, nalbuphine, ketamine, etc. For rapid detection, we developed the automated identification system. It was made up a new software, "DrugMan", modified Chemstation data analysis menu and newly developed macro modules. A series of peak selection, identification and reporting of the results were performed automatically by this system. Concentrations of alcohol in 275 blood samples were ranged from 0.011 to 0.249% (average, 0.119%). Among 149 blood samples, just six samples (4.0%) were showed positive results to the immunoassay: one methamphetamine and five benzodiazepines group I. By GC-MS confirmation, only benzodiazepines were detected and methamphetamine was not detected from immunoassay positive blood sample. Besides these drugs, 5 chlorpheniramines, dextromethorphan, diazepam, doxylamine, ibuprofen, lidocaine and topiramate were also detected in whole bloods by GC-MS. Conclusively, the frequency of drug abuse for Korean drivers was relatively low. There was none case which illegal drug was detected. However these results were limited to alcohol positive blood samples, so it is necessary to analyze more samples including alcohol negative blood.

• Journal of Food Hygiene and Safety
• /
• v.36 no.1
• /
• pp.24-33
• /
• 2021

For this study, we surveyed concentrations of 8 mycotoxins (aflatoxin B1, B2, G1, G2, ochratoxin A, fumonisin B1, B2 and zearalenone) in agricultural products used for food and medicine by liquid chromatography-tandem mass spectrometry and conducted a risk assessment. Samples were collected at the Yangnyeong Market in Seoul, Korea, between January and November 2019. Mycotoxins were extracted from these samples by adding 0.1% formic acid in 50% acetonitrile and cleaned up by using an ISOLUTE Myco cartridge. The method was validated by assessing its matrix effects, linearity, limit of detection (LOD), limit of quantification (LOQ), recovery and precision using four representative matrices. Matrix-matched standard calibration was used for quantification and the calibration curves of all analytes showed good linearity (r2>0.9999). LODs and LOQs were in the range of 0.02-0.11 ㎍/kg and 0.06-0.26 ㎍/kg, respectively. Sample recoveries were from 81.2 to 118.7% and relative standard deviations lower than 8.90%. The method developed in this study was applied to analyze a total of 187 samples, and aflatoxin B1 was detected at the range of 1.18-7.29 ㎍/kg (below the maximum allowable limit set by the Ministry of Food and Drug Safety, MFDS), whereas aflatoxin B2, G1 and G2 were not detected. Mycotoxins that are not regulated presently in Korea were also detected: fumonisin (0.84-14.25 ㎍/kg), ochratoxin A (0.76-17.42 ㎍/kg), and zearalenone (1.73-15.96 ㎍/kg). Risk assessment was evaluated by using estimated daily intake (EDI) and specific guideline values. These results indicate that the overall exposure level of Koreans to mycotoxins due to the intake of agricultural products used for food and medicine is unlikely to be a major risk factor for their health.