摘要
建立了固相萃取-气质联用（GC—MS）法同时快速测定水性胶黏剂中16种邻苯二甲酸酯的分析方法。水性胶黏剂加入去离子水，并用正己烷在超声条件下萃取，取适量萃取液于离心管中离心10min，取上层清液，经Florisil玻璃固相萃取柱净化，用正己烷超声溶解并定容至1mL，进行GC．MS分析，内标法定量。整个分离过程21min即可完成。实验结果表明，16种邻苯二甲酸酯在0．02-1．0mg／L范围内具有良好线性关系（r2〉0．9992），检出限均小于O．01mg／L；在5，10，15mg／kg添加水平，邻苯二甲酸酯的加标回收率在85．4％～111．5％之间，相对标准偏差在0．7％～9．0％之间。方法适合于水性胶黏剂中16种邻苯二甲酸酯的同时检测及确证。
A method for rapid separation and simultaneous determination of 16 phthalate esters in water-borne adhesives was developed by solid phase extraction-gas chromatography-mass spectrometry （GC-MS）. Deionized water was used to extract water-borne adhesives＇, and then n-hexane was used to extract it under ultrasonic condition. Appropriate extract was placed into the centrifuge tube and centrifugated 10 mins, the supernatant was through a glass Florisil SPE column to clean up and volumed to 1 mL by ultrasonic dissolution with n-hexame for GC-MS analysis, and then quantified by the internal standard method. The total separation process was within 21 minutes to be completed. As a result, the calibration curves of 16 phthalate esters were linear in the range of 0. 02 - 1.0 mg/L, with correlation coefficents more than 0. 9992. The recoveries of the spiked samples at the levels of 5, 10, 15 mg/kg were in the range of 85. 4% - 111.5%, withRSDs （n=10） of 0.7% - 9. 0%, all were less than 9.0%. The detection limits of phthalate esters in water-borne adhesives samples were less than 0. 01 mg/L. This method is, suitable for simultaneous detection and confirmation of 16 kinds of phthalates in water-based adhesives.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第5期592-596,共5页
Chinese Journal of Analysis Laboratory
关键词
邻苯二甲酸酯
气相色谱-质谱
固相萃取
水性胶黏剂
测定
Phthalates
Gas chromatography-mass spectrometry （ GC-MS ）
SPE
Waterborne adhesives
Hexane extraction
Determination
