Wei D Y, Wang M L, Guo Z Y, Wang S, Li H L, Zhang H N, Gai P P
Ningbo Univ., Zhejiang, PR China.
J Food Sci. 2009 Jun;74(5):C392-8. doi: 10.1111/j.1750-3841.2009.01183.x.
A GC/MS method was developed and successfully validated for the determination of adipate plasticizers in ham sausage migrated from polyvinylidene chloride (PVDC) packaging film. The sample pretreatment includes liquid extraction, solvent evaporation, and reconstitution before and after solid phase extraction (SPE). For the 5 adipate plasticizers studied, the SPE process with Oasis MAX cartridge showed an extraction efficiency from 85.7% to 106%, and the calibration curves are all linear in the range of 5 to 1000 ng/g with correlation coefficients greater than 0.998. The method proved to be accurate and precise; the average intraday recovery ranges from 85.4% to 114.6% with a %CV value from 2.5 to 11.3, and the average interday recovery from 83.6% to 118.5% with a %CV value from 2.8 to 15.6, respectively, for the adipate plasticizers. The method is sensitive and was effectively applied in the kinetic and penetration studies of the adipate plasticizers migrating from food-grade PVDC packaging film into ham sausage. The experimental data showed that approximately 6.8% of dibutyl adipate (DBA) in the packaging film migrated into the ham sausage in 4 mo and the migration reached the innermost portion of the sausage in 6 mo.
建立了一种气相色谱/质谱（GC/MS）方法，并成功验证了该方法可用于测定从聚偏二氯乙烯（PVDC）包装薄膜迁移至火腿肠中的己二酸酯类增塑剂。样品预处理包括在固相萃取（SPE）前后进行液液萃取、溶剂蒸发和复溶。对于所研究的5种己二酸酯类增塑剂，使用Oasis MAX柱进行的SPE过程萃取效率在85.7%至106%之间，校准曲线在5至1000 ng/g范围内均呈线性，相关系数大于0.998。该方法经证明准确且精密；对于己二酸酯类增塑剂，日内平均回收率在85.4%至114.6%之间，变异系数（%CV）值在2.5至11.3之间，日间平均回收率在83.6%至118.5%之间，%CV值在2.8至15.6之间。该方法灵敏，已有效应用于食品级PVDC包装薄膜中己二酸酯类增塑剂向火腿肠迁移的动力学和渗透研究。实验数据表明，包装薄膜中约6.8%的己二酸二丁酯（DBA）在4个月内迁移至火腿肠中，6个月时迁移至香肠的最内层。
