超高效液相色谱／静电场轨道阱高分辨质谱法快速测定纸质食品接触材料中的5种异噻唑啉酮类防腐剂  

Rapid Determination of Five Isothiazolinone Preservatives in Paper Packaging Materials Intended to Come into Contact with Foodstuffs by UPLC/Orbitrap HRMS

作　　者：王成云[1] 刘彬彬[1] 尹丽娟[1] 林君峰[1] 沈雅雯[2] 

机构地区：[1]深圳出入境检验检疫局,广东深圳518067 [2]深圳大学化学与环境工程学院,广东深圳518060

出　　处：《造纸化学品》2016年第5期24-29,共6页Paper Chemicals

基　　金：深圳出入境检验检疫局科技计划项目（SZ2014102）

摘　　要：建立了一种快速测定纸质食品接触材料中5种异噻唑啉酮类防腐剂的超高效液相色谱／静电场轨道阱高分辨质谱（UPLC／Orbitrap HRMS）分析方法。该方法以甲醇为萃取溶剂，超声萃取纸质食品接触材料中的异噻唑啉酮类防腐剂．萃取液经浓缩定容后，进行UPLC／OrbitrapHRMS分析。采用Hypersil GOLD色谱柱（100mmx2．1mm，1．9μm）对5种异噻唑啉酮类防腐剂进行色谱分离，流动相为甲醇一妒（甲酸）=0．1％水溶液，洗脱方式为梯度洗脱。质谱分析采用电喷雾正离子（ESI＋）模式，一级质谱全扫描范围为m／Z100-300，5种异噻唑啉酮类防腐剂的质量准确度误差均小于2×10^—6。利用目标分析物的保留时间和准分子离子的精确质量数进行定性，利用提取离子色谱峰面积进行外标法定量。在0．2～100．0μg／L范围内，5种异噻唑啉酮类防腐剂的线性相关系数均大于0．998。方法检出限为0．1μg／kg。在3个不同加标浓度水平下，平均加标回收率为81．8％～94．5％，相对标准偏差为3．6％～9．8％。该方法定性可靠，定量准确，检出限低，可完全满足纸质食品接触材料中异噻唑啉酮类防腐剂检测工作的需要。Abstract：An effective method was established for rapid determination of five isothiazolinone preservatives in paper packaging materials intended to come into contact with foodstuffs using ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry （UPLC/Orbitrap HRMS） technique. Isothiazolinone preservatives in paper packaging materials intended to come into contact with foodstuffs were ultrasonically extracted by using methanol as the extraction solvent. The extract was concentrated and analyzed by UPLC/Orbitrap HRMS. The chromatographic separation of five isothiazolinone preservatives was performed on a Hypersil GOLD column（100 mm×2.1 mm, 1.9 μm） with a gradient elution of methanol and 0.1%（volume） aqueous formic acid solution. Five isothiazolinone preservatives were detected by orbitrap HRMS in ESI positive mode. Full-scan experiment was performed in the range from m/Z 100 to m/Z 300. Five isothiazolinone preservatives were routinely detected with mass accuracy error below 2× 10^-6. The qualitative analysis was carried out by the retention time and the exact mass of quasi-molecularion. The quantitative analysis was carried out by the peak area external standards in extracted chromatograms. The correlation coefficients（r） were all larger than 0.998, and the limits of detection （LODs） were 0.1 ~g/kg for all five isothiazolinons in the range from 0.2 ~g/L to 100.0 p.g/L. The blank samples were spiked at three different spiked levels and the spiked average recoveries varied from 81.8% to 94.5% while the relative standard deviation（RSD） varied from 3.6% to 9.8%. The proposed method was reliable, accurate and sensitive, and could completely satisfy the demand on the analysis of isothizolinones in paper packaging materials intended to come into contact with foodstuffs.

关 键 词：超高效液相色谱/静电场轨道阱高分辨质谱 纸质食品接触材料 异噻唑啉酮 超声萃取 快速 测定 

分 类 号：O657.72[理学—分析化学]