摘要
目的建立超高效液相色谱-三重四级杆串联质谱法测定乳粉类产品中5种核苷(腺嘌呤核苷、鸟嘌呤核苷、胞嘧啶核苷、尿嘧啶核苷、次黄嘌呤核苷)和5种核苷酸(胞嘧啶核苷酸、尿嘧啶核苷酸,腺嘌呤核苷酸、次黄嘌呤核苷酸和鸟嘌呤核苷酸)含量的方法。方法样品用温水溶解,经25%乙酸溶液沉淀蛋白后离心,使用T3柱(2.1 mm×100 mm,1.8μm)为分析柱,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液作为流动相,梯度洗脱分离。质谱采用正离子模式,多反应监测模式进行检测,用外标法定量。结果 5种核苷和5种核苷酸在10 min内达到基线分离。次黄嘌呤核苷酸、鸟嘌呤核苷酸在10~1000 ng/m L浓度范围内,其余检测物在5~1000 ng/m L浓度范围内线性关系良好。方法检出限为0.002~0.150 mg/kg,加标回收率为89%~121%,相对标准偏差为0.91%~8.84%(n=6)。结论该方法快速准确、灵敏度高、前处理简单,能够快速测定婴幼儿配方奶粉中5种核苷和5种核苷酸的含量。
Objective To establish a method for the determination of five nueleosides,including adenosine （A）, guanosine （G）, cytidine （C）, uridine （U）, inosine（I） , and five nucleotides, including cytidine monophosphate （CMP） , uridine monophosphate （UMP）, adenosin monophosphate （AMP）, inosme monphosphate （IMP）, guanosine monophosphate （GMP）, from milk powder products by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry （UPLC- MS/MS）. Methods After hydrolysis with warm water, the sample was deproteinated by 25% acetic acid in water. The analysis was performed on a T3 eolmnn （2. 1 mm×100 mm, 1.8 μm） and gradiently eluted using 0. 1% formic acid in both acetonitrile and water as the mobile phase. The samples were determined by mass spectrometry in the positive ion mode with the multiple reaction monitoring mode, quantified by the external standard method. Results Five kinds of nueleosides and five kinds of nucleotides were separated within ten minutes. IMP and GMP were linear in the concentration range of 10 -1000 ng/mL, and the other nucleosides and nucleotides were linear in the concentration range of 5 - 1000 ng/ mL. The limits of detection for five nucleasides and nucleatides were in the range of 0. 002 - 0. 150 mg/kg. Recoveries of five nucleasides and nucleatides at different levels were in ranges of 89% -121% , with the relative standard deviations were in ranges of 0.91% - 8.84% （n = 6）. Conclusion This method is fast, accurate and sensitive and the preprocessing is simple, which can be used for determination of five nucleosides and five nuclestides in milk powder products effectively.
作者
陈曦
张琳
沈葹
Chen Xi;Zhan Lin;Shen Shi(National Institute for Nutrition and Health,Chinese Center for Disease Control and Prevention,Beijing 100050,China)
出处
《卫生研究》
CAS
CSCD
北大核心
2018年第5期804-808,814,共6页
Journal of Hygiene Research
基金
国家自然科学青年基金(No.31501477)
关键词
核苷
核苷酸
奶粉
超高效液相色谱-三重四级杆串联质谱
食品检测
nucleoside
nuclestide
milk powder products
ultra-high performanceliquid chromatography-tandem triple quadrupole mass spectrometry（UPLC-MS/MS）
food detection
