UPLC-MS/MS测定食品及保健食品中酚汀等23种致泻性成分  

Determination of 23 Laxative Ingredients Including Oxyphenisatine in Food and Health-care Food by UPLC-MS/MS

作　　者：张秋炎 罗辉泰 廖均涛 黄芳 梁维维 吴惠勤 ZHANG Qiu-yan;LUO Hui-tai;LIAO Jun-tao;HUANG Fang;LIANG Wei-wei;WU Hui-qin(Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070,China)

机构地区：[1]广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省中药质量安全工程技术研究中心,广东广州510070

出　　处：《分析测试学报》2025年第2期211-220,共10页Journal of Instrumental Analysis

基　　金：广东省科学院打造综合产业技术创新中心行动资金项目(2022GDASZH-2022010110);广东省科学技术厅科技基础条件建设领域专项项目(2024B1212070001)。

摘　　要：建立了同时测定食品及保健食品中非法添加酚汀等23种致泻性成分的超高效液相色谱-串联质谱法(UPLC-MS/MS)。样品经80%甲醇(含0.1%甲酸)提取后,提取液在0.2%甲酸溶液-乙腈的流动相体系下经Agilent Poroshell 120 PFP(2.1 mm×100 mm,2.7μm)色谱柱梯度洗脱分离。采用电喷雾正离子模式下多反应监测(MRM)方式对酚汀等23种致泻性成分进行质谱分析,基质匹配外标法定量。实验表明,酚汀等23种致泻性成分在不同基质(饮料、压片糖果、硬胶囊内容物、果蔬粉、代用茶、酵素梅和果冻)中线性关系良好,相关系数(r)为0.997 1~0.999 9,检出限为0.001~0.5 mg/kg,定量下限为0.002~1.0 mg/kg。饮料、压片糖果、硬胶囊内容物、果蔬粉、代用茶、酵素梅和果冻样品在3个不同加标水平下的平均回收率为77.5%~114%,相对标准偏差为0.81%~12%(n=6)。该法前处理易操作且高效,分析速度快,灵敏度高,定量准确,适用于食品及保健食品中酚汀等23种致泻性成分的同时快速分析。A novel method for the simultaneous and rapid determination of 23 laxative ingredients in⁃cluding oxyphenisatine in various food and health-care food matrices using ultra high performance liq⁃uid chromatography-tandem mass spectrometry(UPLC-MS/MS)has been developed.The different matrix samples were extracted with 80%methanol(containing 0.1%formic acid),and the filtrate was analyzed using an Agilent Poroshell 120 PFP chromatographic column(2.1 mm×100 mm,2.7μm).The mobile phases were 0.2% formic acid aqueous solution and acetonitrile under gradient elution.The mass spectrometry conditions employed an electrospray ionization source and positive ion scan⁃ning with multiple reaction monitoring mode(MRM)for 23 laxative ingredients including oxyphenisat⁃ine.Representative matrices such as drink,tablet candy,hard capsule contents,fruit and vegeta⁃ble powder,substitutional tea,enzymatic plum and jelly samples ware selected.The correlation co⁃efficients(r)for linear calibration curves of 23 laxative ingredients ranged from 0.9971 to 0.9999 in their respective concentration range.The limits of detection(LODs)of 23 laxative ingredients were in the range of 0.001-0.5 mg/kg,and the limits of quantitation(LOQs)were in the range of 0.002-1.0 mg/kg.The recoveries at low,medium and high concentration levels ranged from 77.5%to 114%,with relative standard deviations(n=6)ranged from 0.81%to 12%.The established method is simple,effective,rapid,high sensitive and accurate,making it suitable for the determination of 23 laxative ingredients in food and health-care food.

关 键 词：超高效液相色谱-串联质谱法 食品 保健食品 酚汀 酚酞 致泻性成分 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]