高效液相色谱-质谱法测定橄榄油中β-谷甾醇的含量

Determination of β-sitosterol in olive oil by HPLC-MS

采用皂化法进行样品前处理，高效液相色谱柱进行分离，采用大气压化学电离源（APCI），以正离子检测方式进行质谱分析，外标法定量，建立了液相色谱-质谱（LC—MS）法检测橄榄油中β-谷甾醇含量的方法。实验结果表明，β-谷甾醇质量浓度在5．00～100mg／L范围内与色谱峰面积呈良好的线性关系，相关系数R2=0．9999，检出限为1．00mg／kg。在2个添加水平下，样品的加标回收率为90．1％～96．0％，相对标准偏差为2．1％-4．1％（n=6）。该方法的建立，为橄榄油中β-谷甾醇的检测提供了一种前处理简便、选择性好、灵敏度高的检测方法。

A new method for determining β-sitosterol in olive oil by LC-MS was established in this work. β-sitosterol was estracted from olive oil after saponification, and the extracted solution was determined by HPLC-MS, using C18 reverse phase column and atmospheric pressure chemical ionization （APCI）. External standard was used for quantification. The results showed that the concentration of the 13-sitosterol had good linear relationship with the chromatographic peak area in the range of 5.00～100 mg/L, with correlation coefficient of 0.9999, and detection limit of 1.00 mg/kg. The recoveries under two spiked levels were 90.1%～96.0%, and the relative standard deviations were 2.1%-4.1% （n=6）. The established method provides a method, which has the characteristic of simple pretreatment, good selectivity and high sensitivity, for the detection of β-sitosterol in olive oil. The establishment of the method, which providing a simple and convenient.