超高效液相色谱-串联质谱法检测水系模拟物中11种工业用抗氧化剂  

Determination of 11 industrial antioxidants in the aqueous simulants by ultra-performance liquid chromatographytandem mass spectrometry

作　　者：范赛[1] 邹建宏[2] 李丽萍[1] 张楠[1] 刘伟[1] 李兵[1] 赵旭东[1] 吴国华[1] 薛颖[1] 赵榕[1] 

机构地区：[1]北京市疾病预防控制中心,营养与食品卫生所,科研教学管理办公室,北京100013 [2]中国人民解放军第二炮兵总医院,北京100088

出　　处：《色谱》2014年第9期999-1004,共6页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑计划项目(2011BAK10B05-04)

摘　　要：建立了水系模拟物中11种工业用抗氧化剂的超高效液相色谱-串联质谱检测方法。水系模拟物经ProElut PLS固相萃取柱浓缩富集,采用ACQUITY UPLCTM BEH C18超高效液相色谱柱（100 mm×2.1 mm,1.7μm）分离,水和乙腈作为流动相进行梯度洗脱,电喷雾离子源电离,负离子多反应监测模式下进行监测,外标法定量。11种化合物在5.0-100μg/L范围内呈良好线性关系,相关系数r〉0.995,方法检出限为0.2-1.0μg/L,定量限为0.5-3.0μg/L。5.0、10.0和20.0μg/L添加水平下的加标回收率为61.4%-109.4%,RSD为3.9%-18.2%（n=6）。该方法操作简单、稳定、可靠,可以满足水系模拟物中11种抗氧化剂的定性确证和定量检测。An ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/ MS） method has been developed to identify and determine I I industrial antioxidants in the aqueous simulants. A ProElut PLS SPE column was used for the enrichment, and an ACQUITY UPLCTM BEH C18 UPLC column （ 100 mm×2. 1 mm, 1.7 μm） was used for separation by the gradient elution with pure water and acetonitrile as the mobile phases. The MS/MS detection was performed with an electrospray ionization （ESI） source in negative mode. The external standard method was used for quantitation in the present study. The linear ranges of the 11 analytes were from 5.0 to 100μg/L. The coefficients of correlation were greater than 0. 995. The recoveries of blank aqueous simulants fortified with the 11 analytes at the levels of 5.0, 10.0 and 20.0 μg/L were 61.4% to 109.4% with the relative standard deviations varied from 3.9% to 18.2% （ n = 6 ）. The LODs and LOQs of the 11 analytes in aqueous simulants were 0.2- 1.0 μg/L and 0.5-3.0 μg/L, respectively. This method is highly sensitive and accurate, and can be applied to the determination of the 11 trace industrial antioxidants in the aqueous simulants.

关 键 词：超高效液相色谱-串联质谱 固相萃取 抗氧化剂 水系模拟物 包装材料 

分 类 号：O658[理学—分析化学]