Yamazaki Y, Ninomiya T
Institute of Food Hygiene, Japan Food Hygiene Association, Yaizu, Japan.
J AOAC Int. 1998 Nov-Dec;81(6):1252-6.
A simple and rapid method was developed for determining bitertanol residues in strawberries. Bitertanol was extracted from samples with ethyl acetate. Bitertanol acetate was added prior to extraction as a surrogate standard. The ethyl acetate extract was cleaned up by passing through tandem solid-phase extraction columns consisting of anion-exchange (SAX) and aminopropyl (NH2) bonded silica. The eluate was evaporated to dryness and reconstituted with methanol. Bitertanol residues were determined by liquid chromatography with fluorescence detection. Recoveries at 4 fortified levels (0.05, 0.25, 0.5, and 1.0 microgram/g), calculated by the internal standard method, ranged from 92.1 to 99.1%, with coefficients of variation ranging from 0.3 to 4.0%. The detection limit was 0.01 microgram/g. Of 25 commercial strawberry samples analyzed for bitertanol residues, 5 contained bitertanol residues at concentrations ranging from 0.02 to 0.51 microgram/g. Positive samples were confirmed by gas chromatography/mass spectrometry with mass-selective detection (m/z 170 and 168).
开发了一种简单快速的方法来测定草莓中的联苯三唑醇残留量。用乙酸乙酯从样品中提取联苯三唑醇。在提取前加入乙酸联苯三唑醇作为替代标准物。乙酸乙酯提取物通过由阴离子交换（SAX）和氨丙基（NH2）键合硅胶组成的串联固相萃取柱进行净化。洗脱液蒸发至干，并用甲醇复溶。通过液相色谱-荧光检测法测定联苯三唑醇残留量。采用内标法计算在4个加标水平（0.05、0.25、0.5和1.0微克/克）下的回收率，范围为92.1%至99.1%，变异系数范围为0.3%至4.0%。检测限为0.01微克/克。在分析的25个市售草莓样品中，有5个含有浓度范围为0.02至0.51微克/克的联苯三唑醇残留。阳性样品通过气相色谱/质谱联用的质量选择性检测（m/z 170和168）进行确证。
