超高效液相色谱联用质谱测定食品中磷脂酰胆碱、磷脂酰乙醇胺及磷脂酰肌醇  

Simultaneous determination of phosphatidylcholine, phosphatidyl ethanolamine and phosphatidylinositol in food by UPLC-MS/MS

作　　者：朱丽[1] 杨世添 邓梦雅[1] 谭微 彭祖茂[1] 张协光[1] ZHU Li;YANG Shi-tian;DENG Meng-ya;TAN Wei;PENG Zu-mao;ZHANG Xie-guang(Shenzhen Academy of Metrology and Quality inspection, Shenzhen 518131;Department of Food and Chemical Engineering, Lushan College of Guangxi University of Science and Technology, Liuzhou 545616)

机构地区：[1]深圳市计量质量检测研究院,深圳518131 [2]广西科技大学鹿山学院食品与化学工程系,柳州545616

出　　处：《食品科技》2018年第11期330-335,共6页Food Science and Technology

基　　金：广东省质量技术监督局科技项目(2017CZ12);深圳市计量质量检测研究院科研项目(2016-YA24)

摘　　要：首次建立超高效液相色谱联用质谱法测定食品中磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇的方法。样品经超声提取处理后,用甲醇定容。具体方法为:Hypersil GOLD C18色谱柱(100 mm×2.1 mm,1.9μm),流动相为0.1%(v:v)甲酸水溶液和0.1%(v:v)甲酸甲醇溶液[体积比,(0~1.0)min:85.0%~95.0%;(1.0~7.0)min:95.0%~98.0%;(7.0~12.5)min:98.0%~100%;(12.5~13.0)min:100%~85%;(13.0~15.0)min:85.0%],流速:0.3 mL/min;柱温:30℃;电喷雾离子源,正离子模式,选择反应监测模式扫描,进样量为5μL,外标法定量。3种目标物的线性范围分别为(0.150~15.0)μg/m L、(0.130~13.0)μg/m L、(0.0800~8.00)μg/m L,3种目标物在各自的质量范围内线性关系良好(r>0.9995),3种化合物的检出限为(0.120~3.00)ng/m L,定量限为(1.79~4.71)ng/mL,在3个不同添加水平下的平均回收率为93.2%~98.4%、89.7%~98.0%、94.6%~103%,相对标准偏差(RSD)为1.15%~8.59%(n=3)。该方法灵敏,准确度高,分析时间快,样品稳定性好,适用于食品中磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇的检测。A method for stimultaneous determination of phosphatidylcholine(PC), phosphatidyl ethanolamine(PE) and phosphatidylinositol(PI) by ultra high performance liquid chromatography coupled with mass spectrometry(UPLC-MS/MS) was developed. After saponification, the samples were extracted by methanol. The following conditions have been proven to be suitable for the separation of three analytes: Hypersil GOLD C18 column(100 mm×2.1 mm, 1.9 μm), mobile phase: 0.1% formic acid/water(v:v) and 0.1% formic acid/methanol(v:v) in the gradient elution mode[(0~1.0)min:85.0%~95.0%;(1.0~7.0)min: 95.0%~98.0%;(7.0~12.5)min: 98.0%~100%;(12.5~13.0)min: 100%~85%;(13.0~15.0)min: 85.0%, v/v]. mobile phase rate: 0.3 m L/min, oven temperature: 30 ℃, injection volume: 5 μL, the detection was performed using UPLC-ESI-MS/MS detector with selective reaction monitoring(SRM) in positive mode, external standard method was used for quantification. The correlation coefficients(r) were greater than 0.9995 in the linear ranges of 3 analytes in ranges of(0.150~15.0)μg/m L,(0.130~13.0)μg/m L and(0.0800~8.00)μg/m L, The limits of detection(LODs) were in the range of(0.120~3.00)ng/m L and the limits of quantification(LOQs) were(1.79~4.71)ng/m L. At the three spiked levels, the recoveries were 93.2%~98.4%, 89.7%~98.0%, 94.6%~103%, with the relative standard deviations(RSDs, n=3) ranging from 1.15% to 8.59%. The proposed method is sensitive, accurate and fast, and the samples were in good stable. It is suitable for simultaneous determination of three nutrients in food samples.

关 键 词：磷脂酰胆碱(PC) 磷脂酰乙醇胺(PE) 磷脂酰肌醇(PI) 超高效液相色谱-质谱(UPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学]