Tada Hiroyuki, Nagai Hiroyuki, Shiraki Koichi, Deyashiki Yoshihiro
Gifu Prefectural Research Institute for Health and Environmental Sciences.
Shokuhin Eiseigaku Zasshi. 2008 Jun;49(3):136-40. doi: 10.3358/shokueishi.49.136.
A simplified method for the determination of benzylaminopurine in agricultural products by LC/MS was investigated. Benzylaminopurine in agricultural products was extracted with acetone and the extract was concentrated to below 30 mL. Buffer solution of pH 9.0 and ethyl acetate were added to the residue, and the solution was shaken. The ethyl acetate layer was evaporated to dryness, and the residue was dissolved in acetone-n-hexane (1 : 1). The solution was applied to a SAX/PSA mini-column, which was then rinsed with acetone-n-hexane (1 : 1). Benzylaminopurine was eluted with acetone-n-hexane (1 : 1) containing 1% water. The eluates were evaporated to dryness, and the residue was dissolved in 10 mmol/L ammonium acetate-methanol (1 : 1). Benzylaminopurine was analyzed by LC/MS. The MS detection was performed in the selected ion monitoring (SIM) mode, with detection of the M+H(+) ion of benzylaminopurine (m/z 226) generated by electrospray ionization (ESI). Recoveries of benzylaminopurine from 15 agricultural products were in the range of 83.1-97.2%. The limits of detection (S/N=3) of benzylaminopurine in all samples except green tea and in green tea were 0.0003 and 0.0012 microg/g, respectively.
研究了一种用液相色谱/质谱法测定农产品中苄氨基嘌呤的简化方法。农产品中的苄氨基嘌呤用丙酮提取，提取物浓缩至30 mL以下。向残渣中加入pH 9.0的缓冲溶液和乙酸乙酯，振荡溶液。将乙酸乙酯层蒸发至干，残渣溶于丙酮-正己烷（1:1）。将溶液加到SAX/PSA微型柱上，然后用丙酮-正己烷（1:1）冲洗。苄氨基嘌呤用含1%水的丙酮-正己烷（1:1）洗脱。洗脱液蒸发至干，残渣溶于10 mmol/L乙酸铵-甲醇（1:1）。用液相色谱/质谱法分析苄氨基嘌呤。质谱检测在选择离子监测（SIM）模式下进行，检测通过电喷雾电离（ESI）产生的苄氨基嘌呤的M+H(+)离子（m/z 226）。15种农产品中苄氨基嘌呤的回收率在83.1-97.2%范围内。除绿茶外所有样品及绿茶中苄氨基嘌呤的检测限（S/N=3）分别为0.0003和0.0012 μg/g。
