柱前衍生-超高效液相色谱-串联质谱法测定隐形牙齿矫正材料中13种双酚类物质的溶出水平  

Determination of 13 bisphenols compounds in invisible orthodontics by pre-column derivatization-ultra high performence liquid chromatography-tandem mass spectrometry

作　　者：胡芳[1] 汪军峰 姚佳希 邓媛媛 刘文卫 吴林林 高蓉[2] 余静[2] HU Fang;WANG Junfeng;YAO Jiaxi;DENG Yuanyuan;LIU Wenwei;Wu Linlin;Gao Rong;Yu Jing(Affiliated Stomatological Hospital of Nanjing Medical University,Nanjing 210029;Department of Hygienic Analysis and Detection,School of Public Health,Nanjing Medical University,Nanjing 211166;Wuxi Center for Disease Control and Prevention,Wuxi 214023)

机构地区：[1]南京医科大学附属口腔医院,南京210029 [2]南京医科大学公共卫生学院卫生检验系,南京211166 [3]无锡疾病控制预防中心,无锡214023

出　　处：《分析试验室》2020年第10期1208-1212,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了柱前衍生-UHPLC-MS/MS同时测定隐形牙齿矫正材料中双酚类物质(BPs)在人工唾液中溶出水平的检测方法。浸泡了牙齿矫正材料的人工唾液经乙酸乙酯提取,丹磺酰氯衍生化,采用C18色谱柱,乙腈-0.1%甲酸为流动相,梯度洗脱进行UHPLC分离,电喷雾正离子扫描,多反应监测,内标法定量。13种BPs线性关系良好,线性相关系数(R2)均大于0.998,检出限为2.0~10 pg/m L,定量限为5.0~20 pg/m L。方法的回收率为85.2%~114.7%,日内、日间精密度(RSD)为0.6%~13%。方法可满足隐形牙齿矫正材料中双酚类物质的溶出水平的测定。A method was developed for detemination of bisphenols compounds in invisible orthodontics by precolumn derivatization-ultra high performance liquid chromatography tandem mass spectrometry.The samples were immersed in prepared artificial saliva and bisphenols were extracted with ethyl acetate after two weeks,derivatized by dansyl chloride.The detection and quantification of 13 BPs were performed using LC-MS/MS in ESI+mode.The chromatographic separation was performed on a C18 column using acetonitrile and 0.1%formic acid as the mobile phase.The linear ranges of BPs were 0.05-10 ng/m L,and the correlation coefficients R2 of the standard curve were above 0.998.The limits of quantification were 5.0-20 pg/m L and the limits of detection of the method were 2.0-10 pg/m L.The mean recoveries for BPs were 85.2%-114.7%.The RSDs of intra-day and inter-day precision for BPs were 0.6%-13%.The method was proved to be suitable to evaluate bisphenols compounds in invisible orthodontics.

关 键 词：UHPLC-MS/MS 柱前衍生化 牙齿矫正器 BPs 

分 类 号：O657.63[理学—分析化学]