高效液相色谱-三重四极杆质谱法测定橄榄油中叶绿素铜钠

Determination of chlorophyllin sodium copper saltinolive oil by high performance liquid chromatography-triple quadrupole mass spectrometry

建立了HPLC-MS/MS测定橄榄油中叶绿素铜钠的方法。橄榄油样品经甲醇提取,冷冻离心分层后,采用HPLC-MS/MS法测定。色谱分离选择Agilent Zorbax XDB-C18色谱柱,以甲醇和0. 1%的甲酸水溶液(98:2,V/V)为流动相进行等度洗脱;质谱采用电喷雾正离子扫描方式,选择反应监测扫描,外标法定量。结果表明,在最佳条件下,叶绿素铜钠质量浓度在7. 5~240μg/L范围内线性关系良好,相关系数大于0. 999。检出限为10μg/kg,定量限为40μg/kg。在40,80和400μg/kg 3个水平下进行加标回收实验,回收率为87. 0%~97. 4%,相对标准偏差为1. 6%~4. 3%。方法可用于橄榄油中叶绿素铜钠的快速检测。

A method for the determination of chlorophyllin sodium copper salt in olive oil by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS)was developed.Olive oil samples were extracted with methanol,frozen and centrifuged,and determined by HPLC-MS/MS.Separated on a Agilent Zorbax XDB-C18 column with isocratic elution,the mobile phases were methanol and 0.1%formic acid aqueous solution(98:2,V/V);the positive ion mode and selective reaction monitoring(SRM)mode were used in the analysis,and the analytes were quantified by the external standard method.The results showed that under optimized sample pretreatment,chromatographic and mass spectrometry conditions,chlorophyllin sodium copper salt had a good linear relationship in the range of 7.5-240μg/L,and the correlation coefficient(r)was greater than0.999.The detection limit(LOD)of copper chlorophyll sodium was 10μg/kg and the limit of quantitation(LOQ)was 40μg/kg.The spiked recoveries test was carried out at three concentration levels of 40,80 and 400μg/kg.The recoveries of chlorophyllin sodium copper salt were 87.0%-97.4%,and the relative standard deviations(RSDs)were 1.6%-4.3%(n=6).The method can be used for rapid detection of chlorophyllin sodium copper salt in olive oil.