潲水油中辣椒素检测技术研究

Research on detection technology of capsaicinoids in hogwash oil

目的:建立高灵敏度的潲水油中辣椒素的测定的方法,用于检测甄别潲水油。方法:样品用0.5 mol/L的氢氧化钠溶液振荡提取,反相C18小柱浓缩净化,以乙腈(0.01%甲酸)-0.01%甲酸水溶液为流动相进行梯度洗脱,通过液相色谱-质谱/质谱以MRM方式检测,以二苯胺为内标定量。结果:测定辣椒碱、二氢辣椒碱方法的线性范围均为0.2μg/L～40.0μg/L,线性相关系数分别为0.9997和0.9999,检出限分别为3.2 ng/kg、2.8 ng/kg,回收率分别为87.2%～90.6%、91.9%～102.4%。对39个油样进行检测,对潲水油的鉴别判断正确率为92.3%。结论:方法简便,灵敏度好,选择性好,可作为潲水油的有效鉴别手段。

Objective：To develop a method for determination of capsaicin in hogwash oil with high performance liquid chromatography - mass spectrometry. Methods： The oil sample was extracted by shaking 0.5 mol/L Sodium hydroxide solution and then cleanup was performed on C18 cartridge. The gradient elution was carried out with acetonitrile （0.01% formic acid） -0.01% formic acid as the mobile phase for the baseline separation of the two capsaicinoids in thirty minutes. Diphenylamine was used as internal standard and Multiple Reaction Monitor （MRM） method was applied for detection. Results： The linear range of the two capsaicinoids were all found to be 0.2 μg/L 40.0 μg/L, and the correlation coefficients of the standard curve were 0. 9997 and 0. 9999. The limits of detection were 3.2 ng/kg and 2.8 ng/kg. The recoveries of capsaicin for the spiked samples ranged from 87, 2% to 90.6% and for dihydrocapsaicin ranged from 91.9% - 102.4%. The method was applied for detection of 39 samples and the correct rate was 92.3%. Conculsion ： The HPLC - MS/MS method is suitable for detection of capsaicin and dihydrocapsaicin in hogwash oil and it was proven to be high sensitive and anti -interference.