Bushway R J
Department of Food Science, University of Maine, Orono 04469-5736, USA.
J Chromatogr A. 1996 Nov 22;754(1-2):431-5. doi: 10.1016/s0021-9673(96)00157-4.
The fungicide thiabendazole was quantified in fruit juices and their concentrates (bulk and store bought) without clean-up by simply injecting 50 microliters of dissolved sample into an HPLC. This novel method used a mobile phase consisting of acetonitrile-methanol-water-ethanolamine (37:11:52:0.02) and was passed through a C18 column at 1 ml/min. Detection was accomplished by fluorescence at 305 nm excitation and 345 nm emission. Using peak height thiabendazole was linear from 0.032 to 2.05 ng injected. The limit of quantitation was 5 ppb for juices and store concentrates (2.0 ppb for the limit of detection), 10 ppb for bulk apple concentrates and 25 ppb for other bulk concentrates (5 and 10 ppb, respectively for the limit of detection). Intra- and interassay percent relative standard deviations for standards and samples were mostly below 7% with none above 9%. Eighty-four juices and concentrates out of 200 analyzed were found to contain thiabendazole (2-2560 ppb) by HPLC and all were shown to be thiabendazole positive by enzyme-linked immunosorbent assay (ELISA). The HPLC vs. ELISA correlation coefficient was 0.984.
通过直接将50微升溶解后的样品注入高效液相色谱仪(HPLC),无需净化处理,即可对果汁及其浓缩物(散装和市售)中的杀菌剂噻苯达唑进行定量分析。该新方法采用由乙腈 - 甲醇 - 水 - 乙醇胺(37:11:52:0.02)组成的流动相,以1毫升/分钟的流速通过C18柱。检测通过在305纳米激发波长和345纳米发射波长下的荧光进行。以峰高计算,注入的噻苯达唑在0.032至2.05纳克范围内呈线性关系。果汁和市售浓缩物的定量限为5 ppb(检测限为2.0 ppb),散装苹果浓缩物的定量限为10 ppb,其他散装浓缩物的定量限为25 ppb(检测限分别为5和10 ppb)。标准品和样品的批内和批间相对标准偏差百分比大多低于7%,无一高于9%。通过HPLC分析发现,在200份被分析的果汁和浓缩物中,有84份含有噻苯达唑(2 - 2560 ppb),并且通过酶联免疫吸附测定(ELISA)均显示为噻苯达唑阳性。HPLC与ELISA的相关系数为0.984。