基质辅助激光解吸电离-飞行时间质谱法同时快速测定保健食品中的降压物质  

Simultaneously Analysis of Anti-hypertensive Substances by Matrix-assisted Laser Desorption Ionization Time-of-Flight Mass Spectrometry in Dietary Supplements

作　　者：曾羲 赵甜甜 刘春生 戚平 钱振杰 曹霞飞 王宇 周庆琼[1] 汪宁 Zeng Xi;Zhao Tiantian;Liu Chunsheng;Qi Ping;Qian Zhenjie;Cao Xiafei;Wang Yu;Zhou Qingqiong;Wang Ning(Guangzhou Institute for Food Control,Guangzhou 511400;College of Food Science,South China Agricultural University,Guangdong Provincial Key Laboratory of Food Quality and Safety,Guangzhou 510642;Sericulture&Agri-food Research Institute,Guangdong Academy of Agricultural Sciences,Guangzhou 510610)

机构地区：[1]广州市食品检验所,广州511400 [2]华南农业大学食品学院、广东省食品质量安全重点实验室,广州510642 [3]广东省农业科学院蚕业与农产品加工研究所,广州510610

出　　处：《中国食品学报》2023年第2期288-295,共8页Journal of Chinese Institute Of Food Science and Technology

基　　金：广东省基础与应用基础研究基金项目(2020A 1515010659,2023A1515012605);广东省自然科学基金项目(2019B1515210025);广东省药品监督管理局科技创新项目(2019TDB04);广东省食品质量与安全重点实验室开放基金课题(2021KF003);广州市市场监督管理局科技计划项目(2020kj51)。

摘　　要：建立了基质辅助激光解吸电离-飞行时间质谱(MALDI-TOF MS)同时快速筛查测定盐酸可乐定(HCD)、阿替洛尔(ANL)和利血平(RSP)等3种降压物质的方法。对比了不同点样方式、激光强度对3种药物信号强度的影响等因素,并进行方法学验证。结果表明,以α-氰基-4-羟基肉桂酸(HCCA)为基质,采用混合点样法,反射线性正离子模式下选择激光强度为60%进行MALDI-TOF MS检测时,3个目标物的质谱信号稳定,强度高,响应重复性好。方法学验证结果表明,3种小分子降压物质在10~100 ng/mL线性范围内线性好,相关系数(r)≥0.99,方法的筛查限(LOI)为0.005~0.25μg/g,在液体、固体和半固体3种保健食品基质中的加标回收率为67.56%~104.70%,相对标准偏差(RSDs)为0.43%~10.51%(n=3)。该方法灵敏度好,准确性高,精密度优,抗干扰能力强,有机溶剂消耗少,节能环保,尤其适用于大批量、多批次保健食品中降压物质的检测,填补了传统基质分析筛查保健食品中小分子非法添加物的空白。A matrix-assisted laser desorption ionization time-of-flight mass spectrometry(MALDI-TOF MS)method was set up for simultaneously screening and analysis of 3 kinds of anti-hypertensive substances which is clonidine hydrochloride(HCD),atenolol(ANL)and reserpine(RSP)in dietary supplements.The different spotting approaches and laser power intensities of 3 kinds of anti-hypertensive substances were compared,and the methodology validation experiments were also completed.As a result,α-cyano-4-hydroxycinnamic acid(HCCA)was used as matrix,and samples were spotted by mixed approach under the reflect linear positive mode and laser power of 60%.Under the optinal condition of MALDI-TOF MS,the 3 objectives could obtain stable signals,high intensities and well-repeated mass spectrometrics.The results of method validation showed that the linear relationship was excellent among 10 to 100 ng/mL,and the regression coefficients(r)were all above 0.99.The limit of identification(LOI)were between 0.005 to 0.25μg/g,and the recoveries were in the range of 67.56%-104.70% among liquid,solid and half-solid dietary supplements samples,while the relative standard deviations(RSDs)were ranged from 0.43% to 10.51%(n=3).This method occupied with high sensitivity,accuracy precision,anti-interference ability,low chemical solvents and environmental friendly,which could satisfy multitudinous batches of dietary supplement samples.Meanwhile,this method filled a gap of traditional matrix used in MALDI-TOF MS to screen and analyze small molecule compounds in dietary supplements.

关 键 词：基质辅助激光解吸电离-飞行时间质谱(MALDI-TOF MS) α-氰基-4-羟基肉桂酸(HCCA) 保健食品 降压物质 

分 类 号：TS218[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]