Huang Mingquan

静态顶空-GC/MS技术分析浸膏中的溶剂残留

为研究浸膏类添加剂中的溶剂残留，采用静态顶空进样结合气质联用仪对5种浸膏（枸杞浸膏、山楂浸膏、杭白菊浸膏、茉莉浸膏、桂花浸膏）共15个样品中的27种残留溶剂进行了定性定量分析。静态顶空条件为60℃平衡15 min，进样体积为0.40 mL，利用NIST谱库和标准品定性，外标法定量。结果表明：①该方法对12种溶剂定量的线性范围良好，线性相关系数均大于0.99，回收率在78.60%～120.80%之间，相对标准偏差为11.50%～16.94%。②枸杞浸膏、山楂浸膏、杭白菊浸膏和桂花浸膏（GH1）中的主要残留溶剂为乙醇；桂花浸膏（GH2、GH3）和茉莉浸膏中的主要残留溶剂为甲基环戊烷、正己烷、异己烷和环己烷。

Epoxidation of β-pinene to 2,10-epoxypinane by Oxone

This paper describes a highly effective catalytic method for epoxidation of β-pinene to 2,10-epoxypinane using potassium peroxomonosulfate (Oxone) as oxidant and acetone as catalyst. Structure of 2,10-epoxypinane was characterized by data of infrared spectrum, GC-MS spectrum and 1H NMR spectrum. The procedure consists simply in stirring the substrate, NaHCO3 and acetone, at 0°C, with dropwise addition of an aqueous solution of Oxone. Optimization of the conditions identified (1) the mole ratio of Oxone to β-pinene 0.8:1, (2) reaction temperature 40°C, (3) pH 7.0–7.5, and (4) reaction time 2.5h. The yield of 2,10-epoxypinane can reach 85.4% and the system exhibits good chemical selectivity and few byproducts.