Park Jin-A, Cho Hee-Jung, Cho Soo-Min, Kim Na-Hyun, Kim Dong-Soon, Zhang Dan, Kim Seong-Kwan, Yi Hee, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
Biomed Rep. 2014 Jan;2(1):89-92. doi: 10.3892/br.2013.189. Epub 2013 Oct 29.
The aim of this study was to develop an analytical method for detection of imidocarb [1,3-bis[3-(4,5-dihydro-1h-imidazol-2-yl)phenyl]urea] in beef and milk using high-performance liquid chromatography (HPLC) with diode-array detection (DAD). Imidocarb was separated on a reversed-phase column (4.6×250 mm, 5 μm) with a mobile phase consisting of 85:15 (v/v) 0.1% trifluoroacetic acid/acetonitrile. The flow rate was 1 ml/min, and the column temperature was maintained at 20°C. Detection was carried out at 260 nm using a DAD detector. The analytical samples were extracted using a solid-phase extraction (SPE) method. The calibration curves showed good linearity (r≥0.998). Limits of quantifications (LOQs) were 0.15 mg/kg in beef and 0.025 mg/kg in milk. Intra- and inter-day precisions were 3.2-6.1 and 1.4-6.9%, respectively, and the accuracy (recovery) was 80.4-82.2% and 80.1-89.5% in beef and milk, respectively. Thus, an analytical protocol using SPE extraction followed by HPLC with DAD was successfully developed, which demonstrated acceptable precision and recovery.
本研究的目的是开发一种采用高效液相色谱(HPLC)与二极管阵列检测(DAD)联用的方法,用于检测牛肉和牛奶中的咪唑苯脲[1,3-双[3-(4,5-二氢-1H-咪唑-2-基)苯基]脲]。咪唑苯脲在反相柱(4.6×250 mm,5 μm)上分离,流动相为85:15(v/v)的0.1%三氟乙酸/乙腈。流速为1 ml/min,柱温保持在20°C。使用DAD检测器在260 nm波长处进行检测。分析样品采用固相萃取(SPE)法进行提取。校准曲线显示出良好的线性关系(r≥0.998)。牛肉中的定量限(LOQ)为0.15 mg/kg,牛奶中的定量限为0.025 mg/kg。日内和日间精密度分别为3.2 - 6.1%和1.4 - 6.9%,牛肉和牛奶中的准确度(回收率)分别为80.4 - 82.2%和80.1 - 89.5%。因此,成功开发了一种采用SPE萃取后接HPLC - DAD的分析方法,该方法具有可接受的精密度和回收率。