Asakura Takayuki, Kitamura Mariko, Seki Wataru, Iida Tomonari, Nakazato Mitsuo, Yasuda Kazuo, Nemoto Satoru
Institute for Food and Environment Sciences, Incorporated Foundation Tokyo Kenbikyo-in.
National Institute of Health Sciences.
Shokuhin Eiseigaku Zasshi. 2017;58(4):195-200. doi: 10.3358/shokueishi.58.195.
An LC-MS/MS method for the determination of diniconazole in agricultural products, livestock and marine products was developed. Diniconazole in agricultural products was extracted with acetone. The extract was concentrated and partitioned with n-hexane and 10% sodium chloride solution. Agricultural products such as grains and beans were defatted using n-hexane-acetonitrile. Livestock and marine products were extracted with a mixture of acetone and n-hexane, and the organic layer was evaporated to dryness. The residue was defatted using n-hexane-acetonitrile. Cleanup was carried out using a Florisil cartridge column and a graphitized carbon cartridge column for these samples. The LC separation was carried out on an Inertsil ODS-3 column with a linear gradient of 0.1% formic acid and acetonitrile containing 0.1% formic acid. MS was carried out in the positive ion electrospray ionization mode. The calibration curve was linear between 0.00125 to 0.00750 mg/L. Average recoveries (n=5) of diniconazole from 16 kinds of agricultural products, livestock and marine products fortified at the MRLs (0.01 ppm) were 88.3-108%, and the relative standard deviations were 0.5-5.1%. The limits of quantitation were 0.01 mg/kg.
建立了一种用于测定农产品、畜产品和水产品中烯唑醇的液相色谱-串联质谱法。农产品中的烯唑醇用丙酮提取。提取物浓缩后用正己烷和10%氯化钠溶液进行分配。谷物和豆类等农产品用正己烷-乙腈脱脂。畜产品和水产品用丙酮和正己烷的混合物提取，有机层蒸发至干。残留物用正己烷-乙腈脱脂。使用弗罗里硅土柱和石墨化碳柱对这些样品进行净化。液相色谱分离在Inertsil ODS-3柱上进行，流动相为含0.1%甲酸的0.1%甲酸和乙腈的线性梯度洗脱。质谱采用正离子电喷雾电离模式。校准曲线在0.00125至0.00750 mg/L之间呈线性。在16种农产品、畜产品和水产品中添加烯唑醇的最大残留限量（0.01 ppm），平均回收率（n = 5）为88.3-108%，相对标准偏差为0.5-5.1%。定量限为0.01 mg/kg。
