http://chineseinput.net/에서 pinyin(병음)방식으로 중국어를 변환할 수 있습니다.
변환된 중국어를 복사하여 사용하시면 됩니다.
GC-NPD와 GC-MSD를 이용한 농산물 중 Isotianil의 공정분석법 개발
도정아,이미영,강일현,권기성,오재호 한국분석과학회 2012 분석과학 Vol.25 No.6
Isotianil is a novel fungicide which induces systemic acquired resistance in plants. It has excellent preventive effects as low dosages against rice blast which is one of the most serious diseases in rice. The Maximum Residue Limit (MRL) of Isotianil in republic of korea was set to 0.1 mg/kg in rice, so it is necessary to determine levels of Isotianil residues in agricultural commodities for controlling food safety. Therefore, The purpose of this study was to develop analytical method for the determination of isotiical residues in agricultural commodities using GC-NPD/MSD. Isotianil was extracted with acetonitrile from apple, chinese cabbage, hulled rice, mandarin, pepper, and soybean. The extract was diluted with saline water, and then dichloromethane partition was followed to recover this fungcide from the aqueous phase. A solid phase extraction with Florisil cartridge was additionally employed for final clean up. Isotianil was analyzed and quantitated by GC-NPD and confirmed by GC-MSD. Average recovery of Isotianil ranged from 70.0 to 103.9% in six representative agricultural commodities with relative standard deviations less than 10%, and limit of quantification (LOQ) was 0.05 mg/kg.
도정아,김정연,최지연,이지현,김형주,노은영,조소현,윤창용,김우성 한국분석과학회 2015 분석과학 Vol.28 No.2
Recently, the consumption of dietary supplements has increased because of people’s greater interest in health. Unfortunately, the sales of dietary supplements containing unauthorized substances such as drugs have also increased. We developed a rapid, accurate method for the simultaneous determination of antihistamines using liquid chromatography tandem mass spectrometry with a multiple reaction monitoring mode. The limit of detection (LOD) and limit of quantification (LOQ) of the instrument used in this method were in the ranges 0.0003-0.3 and 0.0009-0.6 μg mL−1, respectively. The linearity of the method was > 0.99. The precision levels of the method were 0.1-9.8% (intra-day) and 0.3-9.6% (inter-day), and the levels of accuracy of the method were 82.7-115.0% (intra-day) and 84.3-113.0% (inter-day). The mean of recovery of the method was in the range of 83.9-117.9% and the RSD of the stability was less than 5.9%.
Determination of streptomycin in kiwifruit samples using LC-ESI-MS/MS
도정아,이미영,조윤제,장문익,홍진환,오재호 한국분석과학회 2015 분석과학 Vol.28 No.4
In May 2012, a safety hazard issue arose because some kiwifruit growers in New Zealand had sprayed streptomycin to prevent kiwifruit canker. Therefore, for food safety management, analytical methods to determine streptomycin residues in kiwifruits are required. We developed an analytical method to determine streptomycin residues in kiwifruit samples using liquid chromatograph tandem mass spectrometer (LC-ESI-MS/MS). Streptomycin residues in samples were extracted using 1% formic acid in methanol, centrifugation for 10 min, and subsequent supernatant filtration. Purified samples were subjected to LC-ESI-MS/MS to confirm presence of and quantify streptomycin residues. Average streptomycin recoveries (6 replicates each sample) were in the range of 94.8%- 110.6% with relative standard deviations of <10%. The linearity of the concentration range of 0.01-5.0 mg/ kg using a matrix-matched calibration gave R2 = 0.9995. The limit of quantification (LOQ) was 0.01 mg/kg. Results showed that our analytical method is rapid, simple, and sensitive, with easy sample preparation.
도정아,노은영,윤순병,박형준,조수열,박성관,윤창용 한국분석과학회 2015 분석과학 Vol.28 No.4
Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatographyquadrupole- time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.
GC-ECD 및 GC-MS를 이용한 현미 중 chloropicrin의 잔류시험법 개발
도정아,최정희,박혜진,박용춘,윤혜정,최동미,오재호 한국식품위생안전성학회 2013 한국식품위생안전성학회지 Vol.28 No.3
A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range 0.005~0.5 μg/mL, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice. Chloropicrin은 국내에서는 사용되지 않으며, 잔류허용기준이 불검출로 설정된 농약이다. 그러나 중국에서는 훈증제, 살균제, 살선충제 및 저장 곡물의 살충제로 사용되고있으며, 잔류허용기준이 설정되어 있다. 따라서 본 연구에서는 중국 등에서 수입하는 식품 중 국내에서 사용하지 않는 농약에 대한 안전성을 확보하기 위하여 해당 농약을 신속하고 빠르게 검출할 수 있는 시험법을 개발하고자 하였다. Chloropicrin은 분자량이 작고 휘발성이 큰 화합물이므로 헤드스페이스 추출법을 활용하여 검체 추출액을 직접GC에 주입하는 시험법을 개발하였으며, 확립된 시험법을검증한 결과 회수율이 77.7~79.3%로 조사되어 코덱스 국제가이드라인(CAC/GL 40)에 적합함을 확인하였다. 정량한계 또한 0.05 mg/kg 이하로 매우 우수한 감도를 가지고있음을 확인하였으며, GC-MS를 이용한 재확인과정을 추가로 확립하여 본 시험법의 신뢰도를 높였다. 확립된 시험법은 식품에 잔류할 수 있는 농약의 기준 준수여부에 대한 적합성을 판단하기 위한 공정시험법으로 활용되고 있다.