食品包装材料中13种增塑剂的毛细管气相色谱法测定

Determination of Thirteen Plasticizers in Food Plastic Packaging Materials by Capillary Column Gas Chromatography

建立了索氏提取、固相萃取净化浓缩、毛细管气相色谱法测定塑料食品包装材料中13种增塑剂的方法。优化了固相萃取淋洗剂、洗脱剂和洗脱剂体积等参数。样品经正己烷索氏提取后，用硅胶小柱净化浓缩。以正己烷一甲苯为淋洗剂，2mL乙酸乙酯为洗脱剂。过滤后的洗脱液用气相色谱仪分析。结果显示，13种增塑剂在0．1～1000mg／L范围内呈良好线性，检出限为0．005～0．030mg／L。样品的加标回收率为90％-116％，相对标准偏差为2．2％-4．9％。

A capillary column gas chromatographic method was developed for the separation and determination of thirteen plasticizers, including dimethyl phthalate acid ester（ DMP）, diethyl phthalate acid ester （ DEP）, dipropyl phthalate acid ester （ DnPP）, diisobutyl phthalate acid ester （ DIBP）, dibutyl phthalate acid ester（DBP）, diamyl phthalate acid ester（ DAP）, bisphenol A（ BPA）, di-n- hexyl phthalate acid ester（DHP）, butyl benzyl phthalate acid ester（BBP）, di-2-ethylhexyl adipate （DEHA）, di（2-ethylhexyl） phthalate acid ester（DEHP）, dioctyl phthalate acid ester（DOP） and dinonyl phthalate acid ester（DNP） in plastic packaging materials for foodstuff. The analytes were extracted with hexane from samples by Soxhlet extraction technique, then purified by silica solid phase extraction. Three key factors such as rinse solvent, eluting solvent and eluting volume were opti- mized. Hexane and toluene （1 ： 1, by volume） were used as rinse solvents, 2 mL ethyl acetate was used as eluting solvent. After filtration, the eluate was determined by gas chromatography with flame ionization detector（GC/FID）. The calibration curves of thirteen plasticizers were linear in the range of 0. 1 - 1 000 mg/L with detection limits of 0. 005 - 0. 030 mg/L. The spiked recoveries ranged from 90% to 116% with relative standard deviations of 2. 2% -4. 9%. The method was successfully applied in the determination of plasticizers in plastic packaging materials for foodstuff.