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《化学分析计量》 2020年第01期
DOI:10.3969/j.issn.1008-6145.2020.01.010
液相色谱-大气压化学电离串联质谱法测定油脂中9 种胆固醇氧化物
丁磊,周典兵,宋伟,吕亚宁,韩芳,郑平
( 合肥海关技术中心,食品安全分析与检测安徽省级重点实验室,合肥 230059) 
Determination of 9 kinds of cholesterol oxides in fats and oils by liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry
DING Lei, ZHOU Dianbing, SONG Wei, LYU Yaning, HAN Fang, ZHENG Ping
(Anhui Entry–Exit Inspection and Quarantine Bureau, Hefei 230059, China; Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230059, China) 
摘要:建立一种准确测定油脂中9 种胆固醇氧化物含量的同位素稀释液相色谱-串联质谱测定方法。向油脂 样品中加入无水乙醇和60% 氢氧化钾溶液,在室温下避光皂化22 h,使用乙醚-石油醚混合液(1∶1)作为提取溶液, 采用液-液萃取方式提取目标物,再使用硅胶柱进行净化,采用5 mmol/L 乙酸铵溶液与甲醇-乙腈混合液(1∶1) 为双流动相梯度淋洗,使用Agilent ZORBAX SB-C18色谱柱分离,在大气压化学电离(APCI)正离子模式下,采用多 反应监测模式内标法定量测定。在10~500 μg/L 范围内,9 种胆固醇氧化物的质量浓度与色谱峰面积线性良好,相 关系数(r2)均大于0.995,检出限均为0.5 mg/kg,在1,5 mg/kg 两个添加水平时,加标回收率为71.2%~94.4%,相 对标准偏差小于10%(n=6)。该方法满足动植物油脂中胆固醇氧化物含量测定需要。 
Abstract:A new method of HPLC-MS/MS for the analysis of nine cholesterol oxides in oil was developed. The oil samples were saponified in dark for 22 h at room temperature by adding anhydrous ethanol and 60% potassium hydroxide solution. With ether-petroleum ether solution (1∶1) as the extraction solution, liquid-liquid extraction method was used to extract the target substance, then silica gel column was used for purification, and 5 mmol/L ammonium acetate and methanol-acetonitrile solution (1∶1) as the mobile phase, atmospheric pressure under the positive ion mode of APCI, the internal standard method of multi reaction monitoring mode was used for quantitative determination. The contents of nine cholesterol oxides had linear relationship with the chromatograph peak areas in the range of 10-500 μg/L with the linear correlation coefficients (2) more than 0.995, and the detection limits were all 0.5 mg/kg. At the addition level of 1 and 5 mg/kg, the recovery rates were 71.2%-94.4% with the relative standard deviation was less than 10% (n=6). This method is suitable for the accurate determination of nine oxides of cholesterol in oil. 
关键词:油脂;胆固醇氧化产物;液相色谱-串联质谱法 
Keywords:oil; cholesterol oxidation products; LC-MS/MS 
基金:安徽检验检疫局科技计划项目(AHKT-01-2017) 
本文引用格式:
丁磊,周典兵,宋伟,等. 液相色谱- 大气压化学电离串联质谱法测定油脂中9 种胆固醇氧化产物[J]. 化学分析计量,2020,29(1):40-44.
DING L,ZHOU D B,SONG W,et al. Determination of 9 kinds of cholesterol oxidation products in fats and oils by liquid chromatographyatmospheric pressure chemical ionization tandem mass spectrometry[J]. Chemical analysis and meterage,2020,29(1):40-44. 

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