Bushway R J, Li L, Paradis L R, Perkins L B
University of Maine, Department of Food Science, Orono 04469-5736.
J AOAC Int. 1995 May-Jun;78(3):815-20.
A liquid chromatographic method has been developed for analysis of the fungicide thiabendazole (TBZ) in fruits, potatoes, and their processed products. Extraction was performed in a 50 mL polyethylene conical centrifuge tube with a basic solution. TBZ was partitioned into methylene chloride with a polytron. No further cleanup was needed. Separation was carried out on a 5 microns Ultracarb 30 ODS column with fluorescent detection, excitation at 305 nm and emission at 345 nm. Total analysis time including extraction was 25 min per sample. Recoveries ranged from 77 to 135%. Average percent recovery for all sample types spiked from 5 ppb to 387 ppm was 94% with a coefficient of variation (CV) of 11%. Overall intra-assay CVs varied from 1.8 to 23%, and interassay CVs ranged from 1.8 to 15%. Of 194 commercial samples analyzed for TBZ, 129 were positive. TBZ in positive samples ranged from 1.1 ppb to 72.5 ppm. The limit of quantitation varied from 2.5 ppb for juices, 2.5 ppb for fruits and potatoes, and 4.5 ppb for bulk concentrates. Detection limits were 1.0 ppb for juice, fruits, and potatoes and 2 ppb for bulk concentrates. TBZ levels in the positive samples were corroborated by immunoassay.
已开发出一种液相色谱法,用于分析水果、土豆及其加工产品中的杀菌剂噻菌灵(TBZ)。在50 mL聚乙烯锥形离心管中用碱性溶液进行萃取。用匀浆器将TBZ分配到二氯甲烷中。无需进一步净化。在5微米的Ultracarb 30 ODS柱上进行分离,采用荧光检测,激发波长为305 nm,发射波长为345 nm。包括萃取在内,每个样品的总分析时间为25分钟。回收率在77%至135%之间。所有加标浓度从5 ppb到387 ppm的样品类型的平均回收率为94%,变异系数(CV)为11%。整体批内CV在1.8%至23%之间,批间CV在1.8%至15%之间。在分析的194个TBZ商业样品中,129个呈阳性。阳性样品中的TBZ含量在1.1 ppb至72.5 ppm之间。定量限因样品类型而异,果汁为2.5 ppb,水果和土豆为2.� ppb, 散装浓缩物为4.5 ppb。果汁、水果和土豆的检测限为1.0 ppb,散装浓缩物的检测限为2 ppb。阳性样品中的TBZ水平通过免疫测定得到证实。