硫酸酸化-气相色谱-质谱法测定植物提取物中的4种多环芳烃

Determination of 4 Polycyclic Aromatic Hydrocarbons in Plant Extract by GC-MS Combined with Sulfuric Acid Acidifaction

5.000g样品经25mL环己烷超声提取两次,提取液浓缩定容至5mL后,采用硫酸(80+20)溶液酸化处理,溶液过0.2μm滤膜后在HP-5MS色谱柱上分离,质谱分析中采用电子轰击离子源和选择离子监测模式。4种多环芳烃的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)为0.13~1.0μg·kg^(-1)。加标回收率为84.2%~105%,测定值的相对标准偏差(n=6)为1.4%~3.9%。方法用于分析10种植物提取物,4种多环芳烃的总质量比在19.59~142.69μg·kg^(-1)之间。

The sample （5. 000 g） was extracted ultrasonically with 25 mL of cyclohexane for two times, then the extract was concentrated to 5 mL and was acidized with sulfuric acid （80＋20） solution. After being filtred by 0. 2μm filter membrane, the solution was separated on a HP-SMS chromatographic column. Electron impact ion source and selected ion monitoring mode were adopted in MS analysis. Linear relationships were found between the peak areas and the mass concentrations of 4 polycyclic armatic pydrocarbons in definite ranges, with detection limits in the range （3S/N） of 0. 13-- 1.0 μg · kg ^-1. Recovery rates obtained by standard addition method ranged from 84. 2% to 105% and RSDs （n=6） ranged from 1.4% to 3. 9%. The method was applied to analysis of 10 plant extracts, giving total mass ratio of 4 polycyclic aromatic hydrocarbons in the range of 19.59--142.69μg · kg^-1.