液相色谱-串联质谱法测定婴儿乳粉中的抗坏血酸棕榈酸酯  

Determination of ascorbyl palmitate in infant formula milk powder by liquid chromatography-tandem mass spectrometry

作　　者：邹芸 张雷 郗存显 刘贝 张后兵 宁莘稀 唐柏彬 ZOU Yun;ZHANG Lei;XI Cun-Xian;LIU Bei;ZHANG Hou-Bing;NING Xin-Xi;TANG Bo-Bin(Chongqing Municipal&Environmental Sanitation Monitoring Departmenty Chongqing 401121,China;The Technology Center of Chongqing Customs,Chongqing 400020,China)

机构地区：[1]重庆市市政环卫监测中心,重庆401121 [2]重庆海关技术中心,重庆400020

出　　处：《食品安全质量检测学报》2021年第1期269-275,共7页Journal of Food Safety and Quality

基　　金：“十三五”国家重点研发计划专项(2016YFD0401105)。

摘　　要：目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)快速检测婴儿乳粉中抗坏血酸棕榈酸酯含量的方法。方法样品经0.1%草酸乙醇溶液提取,提取液用乙二胺-N-丙基硅烷(primary secondary amine,PSA)净化后经C_(18)柱分离,三重四极杆串联质谱检测。结果抗坏血酸棕榈酸酯在0.02-0.5μg/mL浓度范围内与峰面积呈良好的线性关系,相关系数(r^(2))为0.9996,检出限(S/N=3)为0.03 mg/kg,定量限(S/N=10)为0.10 mg/kg。当添加浓度水平为0.5、1.0和10.0 mg/kg时,平均回收率为90.0%~104.1%,相对标准偏差(relative standard deviations,RSDs,n=6)为1.5%~2.7%。结论本方法操作简便、快速、灵敏度高,能够满足婴儿乳粉中抗坏血酸棕榈酸酯的检测要求。Objective To establish a method for rapid detection of ascorbyl palmitate in infant milk powder by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The sample was extracted with 0.1%oxalic acid ethanol solution,and the extract was purified with ethylenediamine-N-propyl silane(primary secondary amine,PSA)and separated by a C_(18)column,and detected by a triple quadrupole tandem mass spectrometry.Results Ascorbyl palmitate had a good linear relationship with the peak area in the concentration range of 0.02-0.5μg/mL,and the correlation coefficient(r^(2))was 0.9996.The limit of detection(LOD)(S/N=3)was 0.03 mg/kg,and the limit of quantitation(LOQ)(S/N=10)was 0.10 mg/kg.The mean recoveries at spiked levels of 0.5,1.0 and 10.0 mg/kg were 90.0%-104.1%,with the relative standard deviations(RSDs)of 1.5%-2.7%(n=6).Conclusion This method is simple,rapid and sensitive,and can meet the requirements of detecting ascorbic palmitate in infant milk powder.

关 键 词：抗坏血酸棕榈酸酯 液相色谱-串联质谱法 婴儿乳粉 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]