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以R (- ) /S (+) 4 (N ,N dimethylaminosulfonyl) 7 (3 iso thiocyanatopyrrolidino) 2 ,1,3 benzoxadiazole(DBD PyNCS)为手性荧光衍生化试剂 ,用反相高效液相色谱法 (RP HPLC)对 DL 肾上腺素对映体进行分离。衍生化反应是在含有 7%吡啶的溶剂中 ,6 5℃温度条件下反应 35min ,生成具有荧光特性的肾上腺素非对映体衍生物(λex=4 6 0nm ,λem=5 5 0nm)。生成的非对映体衍生物在流动相为乙腈 水 (体积比为 2 8∶72 ) ,流速为 1 0mL/min时 ,在DiamonsilTMC18色谱柱 (15 0mm× 4 6mmi d ,5 μm)上分离度可达 2 6。肾上腺素对映体在 0 0 7g/L～ 0 5 0g/L时与峰面积呈良好的线性关系 (r =0 9995 ) ,峰面积测定结果的相对标准偏差为 4 3% (n =7) ,最低检测限为12ng/L(S/N =3)。
The chiral fluorescent derivatization reagent was R (-) / S (+) 4 (3 iso thiocyanatopyrrolidino) 2, 1,3 benzoxadiazole (DBD PyNCS) and was characterized by reverse phase high performance liquid chromatography RP HPLC) to separate the DL adrenaline enantiomer. The derivatization reaction was carried out in a solvent containing 7% pyridine at 65 ℃ for 35 min to generate the adrenaline diastereoisomer derivative (λex = 460nm, λem = 550nm). The resulting diastereomeric derivatives were resolved on a Diamonsil TMMC 18 column (150 mm × 4 6 mm id, 5 μm) using a mobile phase of acetonitrile in a volume ratio of 2: 8: 72 at a flow rate of 10 mL / min Up to 2 6. The enantiomer enantiomer showed a good linear relationship with the peak area (r = 0 9995) at 0 0 7 g / L to 0 0 0 0 g / L, and the relative standard deviation of peak area was 43% (n = 7) , The lowest detection limit of 12ng / L (S / N = 3).