Ishihara Michiyo, Fujita Kazuhiro, Ito Hironobu, Matsuda Takahiro, Yatsukawa Yoh-ichi, Nakamura Munetomo, Sakai Takatoshi, Nemoto Satoru
Japan Food Research Laboratories, Ibaraki-shi, Osaka, Japan.
Shokuhin Eiseigaku Zasshi. 2011;52(5):304-8. doi: 10.3358/shokueishi.52.304.
A novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the trace residue determination of vedaprofen (VPF) in livestock products and seafoods. VPF was extracted from each sample with acidified acetone, and the crude extract was re-extracted with ethyl acetate and NaCl solution. Clean-up was performed using a weak anion exchange cartridge (Bond Elut DEA). The LC separation was performed on a C18 column using acetonitrile-0.0025 mol/L formic acid (3 : 2) as the mobile phase and MS was run in the negative ion electrospray ionization mode. The calibration curve was linear in the range of 0.001-0.1 µg/mL VPF. The mean recoveries from equine muscle, cattle muscle, cattle liver, cattle fat, salmon, eel, corbicula, milk, egg and buckwheat honey were 72-94%, and the relative standard deviations (RSDs) were 1.1-2.0%. Limits of quantitation (LOQs) ranged from 0.001 to 0.007 µg/g.
建立了一种用于测定畜产品和海产品中维达洛芬（VPF）痕量残留的新型液相色谱 - 串联质谱（LC - MS/MS）方法。用酸化丙酮从每个样品中提取VPF，粗提物再用乙酸乙酯和氯化钠溶液进行萃取。使用弱阴离子交换柱（Bond Elut DEA）进行净化。在C18柱上进行LC分离，以乙腈 - 0.0025 mol/L甲酸（3∶2）作为流动相，MS在负离子电喷雾电离模式下运行。校准曲线在0.001 - 0.1 μg/mL VPF范围内呈线性。马肌肉、牛肌肉、牛肝脏、牛脂肪、三文鱼、鳗鱼、蚬、牛奶、鸡蛋和荞麦蜂蜜中的平均回收率为72 - 94%，相对标准偏差（RSD）为1.1 - 2.0%。定量限（LOQ）范围为0.001至0.007 μg/g。
