食品接触用塑料产品中19种邻苯二甲酸酯类增塑剂GC-MS检测研究
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摘要
研究建立了食品接触用塑料产品中19种邻苯二甲酸酯类增塑剂的气相色谱-质谱联用仪(GC-MS)法快速检测方法。塑料产品以正己烷为萃取溶剂,采用超声萃取法对产品中邻苯二甲酸酯类增塑剂进行萃取,萃取液浓缩过滤后进行测定。19种邻苯二甲酸酯类增塑剂在0.05~1mg/L、0.5~10mg/L范围内线性良好,方法检出限(MDL)为0.1238mg/kg~0.9714mg/kg,加标回收率为89.6%~112.9%,相对标准偏差(RSDs)为2.61%~6.36%。该方法重现性好,检出限低,检测结果准确,可用于食品接触用塑料产品中19种邻苯二甲酸酯类增塑剂含量的检测,为食品接触材料中邻苯二甲酸酯质量控制提供相应的技术支撑。
The method for the determination of 19 phthalate plasticizers in plastic products for food contact is developed by gas chromatography-mass spectrometry(GC-MS). The sample is extracted with n-hexane by ultrasonic extraction method and the extract is concentrated and filtered before detection.the calibration curves have a good linear relationship in the range of 0.05~1 mg/L and 0.5~10 mg/L for 19 kinds of phthalate plasticizers. The method detection limit(MDL) is 0.1238 mg/kg~0.9714 mg/kg, its recovery rate is between 89.6%~112.9% with the relative standard deviations(RSDs) of 2.61%~6.36%. The method has good reproducibility and low detection limit, which can be used for the detection of 19 kinds of phthalate plasticizer in plastic products for food contact. It provides technical support for the quality control of phthalate plasticizers in food contact materials.
The method for the determination of 19 phthalate plasticizers in plastic products for food contact is developed by gas chromatography-mass spectrometry(GC-MS). The sample is extracted with n-hexane by ultrasonic extraction method and the extract is concentrated and filtered before detection.the calibration curves have a good linear relationship in the range of 0.05~1 mg/L and 0.5~10 mg/L for 19 kinds of phthalate plasticizers. The method detection limit(MDL) is 0.1238 mg/kg~0.9714 mg/kg, its recovery rate is between 89.6%~112.9% with the relative standard deviations(RSDs) of 2.61%~6.36%. The method has good reproducibility and low detection limit, which can be used for the detection of 19 kinds of phthalate plasticizer in plastic products for food contact. It provides technical support for the quality control of phthalate plasticizers in food contact materials.
引文
[1]张丽丽;陈焕文;李建强;吴转璋;郇延富,邻苯二甲酸酯类化合物检测方法研究进展.理化检验(化学分册)2011,47,(02),241-247.
[2]张建江;舒为群,邻苯二甲酸酯雌性生殖毒性研究进展.卫生研究2005,34,(4),496-498.
[3]Hauser,R.;Meeker,J.D.;Duty,S.;Silva,M.J.;Calafat,A.M.,Altered semen quality in relation to urinary concentrations of phthalate monoester and oxidative metabolites.Epidemiology 2006,17,(6),682-691.
[4]Schettler,T.E.D.,Human exposure to phthalates via consumer products.International journal of andrology2006,29,(1),134-139.
[5]Tyl,R.W.;Myers,C.B.;Marr,M.C.;Fail,P.A.;Seely,J.C.;Brine,D.R.;Barter,R.A.;Butala,J.H.,Reproductive toxicity evaluation of dietary butyl benzyl phthalate(BBP)in rats.Reproductive toxicology 2004,18,(2),241-264.
[6]GB 9685-2016《食品安全国家标准食品接触材料及制品用添加剂使用标准》[S].国家卫生和计划生育委员会.中国标准出版社
[7]GB 31604.30-2016《食品安全国家标准食品接触材料及制品邻苯二甲酸酯的测定和迁移量的测定》[S].国家卫生和计划生育委员会.中国标准出版社
2 DEP 149 177,105 12 DBEP 149 101,85
3 DAP 149 41,132 13 DCHP 149 167,249
4 DIBP 149 223,104 14 DEHP 149 167,279
5 DBP 149 223,205 15 DPh P 225 77,104
6 DMEP 149 59,104 16 DNOP 149 279,104
7 BMPP 149 167,85 17 DNP 149 293,167
8 DEEP 149 72,104 18 DIDP 307 149,141
10 DHXP 149 251,104 9 DPP 149 237,219 19 DINP 293 149,127Tab.2 The content of DEHP in plastic extracted by different solvents表2不同溶剂萃取塑料包装后测得的DEHP量萃取溶液正己烷丙酮乙酸乙酯二氯甲烷甲醇DEHP峰面积4157 3825 4150 3705 3213
2 结果与讨论2.2萃取时间的选择2.1溶剂的选择每次萃取30min,收集萃取液进行浓缩后测定,考察不同超声萃取时间对萃取结果的影响,
[2]张建江;舒为群,邻苯二甲酸酯雌性生殖毒性研究进展.卫生研究2005,34,(4),496-498.
[3]Hauser,R.;Meeker,J.D.;Duty,S.;Silva,M.J.;Calafat,A.M.,Altered semen quality in relation to urinary concentrations of phthalate monoester and oxidative metabolites.Epidemiology 2006,17,(6),682-691.
[4]Schettler,T.E.D.,Human exposure to phthalates via consumer products.International journal of andrology2006,29,(1),134-139.
[5]Tyl,R.W.;Myers,C.B.;Marr,M.C.;Fail,P.A.;Seely,J.C.;Brine,D.R.;Barter,R.A.;Butala,J.H.,Reproductive toxicity evaluation of dietary butyl benzyl phthalate(BBP)in rats.Reproductive toxicology 2004,18,(2),241-264.
[6]GB 9685-2016《食品安全国家标准食品接触材料及制品用添加剂使用标准》[S].国家卫生和计划生育委员会.中国标准出版社
[7]GB 31604.30-2016《食品安全国家标准食品接触材料及制品邻苯二甲酸酯的测定和迁移量的测定》[S].国家卫生和计划生育委员会.中国标准出版社
2 DEP 149 177,105 12 DBEP 149 101,85
3 DAP 149 41,132 13 DCHP 149 167,249
4 DIBP 149 223,104 14 DEHP 149 167,279
5 DBP 149 223,205 15 DPh P 225 77,104
6 DMEP 149 59,104 16 DNOP 149 279,104
7 BMPP 149 167,85 17 DNP 149 293,167
8 DEEP 149 72,104 18 DIDP 307 149,141
10 DHXP 149 251,104 9 DPP 149 237,219 19 DINP 293 149,127Tab.2 The content of DEHP in plastic extracted by different solvents表2不同溶剂萃取塑料包装后测得的DEHP量萃取溶液正己烷丙酮乙酸乙酯二氯甲烷甲醇DEHP峰面积4157 3825 4150 3705 3213
2 结果与讨论2.2萃取时间的选择2.1溶剂的选择每次萃取30min,收集萃取液进行浓缩后测定,考察不同超声萃取时间对萃取结果的影响,