气相色谱–质谱联用法测定油用牡丹花蕊和花粉中角鲨烯含量

Determination of Squalene in Peony Stamen and Pollen for Oil by Gas Chromatograph–Mass Spectrometry

建立气相色-谱质谱联用（GC-MS）测定油用牡丹花蕊及花粉中角鲨烯含量的方法。牡丹花蕊及花粉经索氏抽提法提取脂肪后，用氢氧化钾-乙醇溶液皂化，石油醚萃取净化，正己烷溶解，提取物经HP-5MS柱分离后进入质谱仪检测，外标法定量。结果表明：油用牡丹花蕊和花粉中角鲨烯含量分别为2．73，1．75g／kg。在0．08-400mg／L范围内角鲨烯含量与定量离子m／z69的峰面积线性相关，相关系数为0．9996，方法的检出限为11ng／kg。在1．00-3．00g／kg范围内进行加标回收试验，平均回收率为92．5％～102．6％，测定结果的相对标准偏差为3．4％～5.3（n=6）。该方法具有较好的准确性和重复性，适用于油料植物和植物油中角鲨烯含量的测定。

A method for quantitative of squalene in peony stamen and pollen for oil was determined by GC-MS. The peony stamen and pollen oil was extracted by Soxhlet extraction. The extracted oil samples were saponified with potassium hydroxide-ethanol solution, extracted with petroleum ether and dissolved with n-hexane. The extracted solutions were separated on a HP-5MS column and determined with mass spectrometer. The squalene content in oil peony stamen and pollen were 2.73 and 1.75 g / kg. The contents of squalene had good linear relationship in the range of 0.08-400 mg / L with the peak area of quantitative ion m/z 69, and the correlation coefficient reached 0.999 6. The method of detection limit was 11 ng/ kg. The recoveries of squalene ranged from 92.5% to 102.6% at fortification levels of 1.00-3.00 g/kg, and the relative standard deviation was 3.4%-5.3%（n=6）. This method has good accuracy and repeatability which can be applied to the determination of squalene in oil plants and vegetable oil.