固相萃取-气相色谱-串联质谱法测定运动饮料中的9种紫外线稳定剂

Determination of Ultra Violet Stabilizers Residues in Sports Beverages Using Solid Phase Extraction in Combination with Gas Chromatography-Tandem Mass Spectrometry

建立了同时测定运动饮料中9种紫外线稳定剂残留量的气相色谱-串联质谱（ GC-MS/MS）方法。采用反相的HLB固相萃取柱,对样品中的9种目标物进行萃取、富集、净化。样品试液经气相色谱分离后,采用三重四级杆质谱的多反应监测模式（ MRM）进行测定,外标法定量。在一定浓度范围内,9种紫外线稳定剂的浓度与峰面积的线性关系良好,相关系数均大于0.997。方法检出限为0.03~2.0μg/kg；定量限为0.08~5μg/kg。空白运动饮料样品加标浓度水平为0.005,0.05和0.2 mg/kg时,平均回收率为66.7%~107.3%；相对标准偏差为3.2%~13.8%。经验证,本方法适用于运动饮料中9种紫外线稳定剂残留的同时检测。

A gas chromatography-tandem mass spectrometric （ GC-MS/MS ） method was established for the simultaneous determination of 9 ultra violet （ UV） stabilizer residues in sports beverages. The reversed-phase HLB solid phase extraction cartridges were used for the extraction, enrichment and clean-up of the analytes in the beverages. The samples were separated on a Rtx？-5 column, and subsequently determined by triple quadruple mass spectrometry working in the multiple reaction monitor mode. The quantification was achieved by external standard method. There were good linear correlations between the peak areas and concentration of the 9 UV stabilizers, and the correlation coefficients were above 0. 997. The limits of detection （LOD） of the studied UV stabilizers were in the range of 0. 03-2. 0 μg/kg, and the limits of quantification （LOQ） were in the range of 0. 08-5. 0μg/kg. The mean recoveries were from 66. 7% to 107. 3%, at spiked levels of 0. 005, 0. 05 and 0. 2 mg/kg, and the relative standard deviations （ RSD） were between 3. 2% and 13. 8%. The method was successfully applied to the analysis of multiple UV stabilizer residues in sports beverages.