超声提取–气相色谱–质谱法测定塑料包装食品中16种邻苯二甲酸酯类增塑剂
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摘要
建立超声提取–气相色谱–质谱法同时测定塑料包装食品中16种邻苯二甲酸酯类增塑剂的残留量。以甲醇为萃取溶剂,采用超声萃取法进行样品处理,超声提取时间为30 min,超声提取温度为50℃。16种邻苯二甲酸酯类物质的质量浓度在0.1～50 mg/L范围内与峰面积具有良好的线性关系,线性相关系数均大于0.99,方法检出限为0.05 mg/L。样品的加标回收率为83.4%～97.0%,测定结果的相对标准偏差为1.91%～4.64%(n=6)。该方法简单、灵敏且准确,适用于塑料包装食品中16种邻苯二甲酸酯类增塑剂残留量的测定。
A method for simultaneous determination of 16 phthalate ester plasticizers residues in plastic packaged foods by ultrasonic extraction–gas chromatography–mass spectrometry(GC–MS) was established. Methanol was used as extraction solvent, and ultrasonic extraction pretreatment technology was used to preatreate the sample. The extraction time was 30 minutes and the extraction temperature was 50 ℃. The mass concentration of 16 phthalates had good linear relationships with peak area in the range of 0.1–50 mg/L. The linear correlation coef?cients were more than 0.99, and the detection limits were 0.05 mg/L. The recoveries of the samples were 83.4%–97.0%, and the relative standard deviations of the results were 1.91%–4.64%(n=6). The method is simple, sensitive and accurate. It is suitable for the determination of 16 phthalate ester plasticizers residues in plastic packaged foods.
A method for simultaneous determination of 16 phthalate ester plasticizers residues in plastic packaged foods by ultrasonic extraction–gas chromatography–mass spectrometry(GC–MS) was established. Methanol was used as extraction solvent, and ultrasonic extraction pretreatment technology was used to preatreate the sample. The extraction time was 30 minutes and the extraction temperature was 50 ℃. The mass concentration of 16 phthalates had good linear relationships with peak area in the range of 0.1–50 mg/L. The linear correlation coef?cients were more than 0.99, and the detection limits were 0.05 mg/L. The recoveries of the samples were 83.4%–97.0%, and the relative standard deviations of the results were 1.91%–4.64%(n=6). The method is simple, sensitive and accurate. It is suitable for the determination of 16 phthalate ester plasticizers residues in plastic packaged foods.
引文
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[3]王守法,周耀斌,宁啸骏,等.气相色谱–质谱法测定婴幼儿乳粉中16种邻苯二甲酸酯类迁移物[J].包装与食品机械,2013,31(6):61–64.
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[10]王新豫,凌镇浩.开放式超声微波协同萃取测定PVC塑料中邻苯二甲酸酯类增塑剂研究[J].化学试剂,2009,31(2):109–111.
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[12]李波平,林勤保,宋欢,等.快速溶剂萃取–高效液相色谱测定塑料中邻苯二甲酸酯类化合物[J].应用化学,2008,25(1):63–66.
[13]张泽明,张洪海,李建龙,等.固相微萃取–气相色谱–质谱联用测定海水与沉积物中邻苯二甲酸酯类污染物[J].分析化学,2017,32(3):348–356.
[14]樊继彩,王姝婷,黄希汇,等.食用油中20种邻苯二甲酸酯的超高效液相色谱–质谱联用法测定[J].中国卫生检验杂志,2013(5):1 063–1 067.
[15]刘晓毅,蒋可心,石维妮,等.国内外食品接触材料中邻苯二甲酸酯类塑化剂迁移限量对比分析[J].食品工业科技,2011(10):397–399.
[16]张明明,刘玉兰,杨金强,等.油脂中邻苯二甲酸酯类塑化剂的吸附脱除研究[J].粮油食品科技,2015,23(5):32–36.
[2]周松华,林勤保,李波,等.气相色谱–质谱联用检测聚丙烯食品包装材料中的18种有毒有害物质[J].包装与食品机械,2015,33(1):56–61.
[3]王守法,周耀斌,宁啸骏,等.气相色谱–质谱法测定婴幼儿乳粉中16种邻苯二甲酸酯类迁移物[J].包装与食品机械,2013,31(6):61–64.
[4]周颖,安莹,曾惠琴.基质分散固相萃取–气质联用法测定含油食品中DBP、BBP、DEHP三种增塑剂含量[J].食品与发酵科技,2018,54(1):21–25.
[5]司腾飞,于江,许彦阳,等. GC/MS测定蒸煮包装袋中DEHP对玉米的迁移量[J].包装工程,2014,35(11):1–5.
[6]何凤飞,陈昌云,陆国飞.毛细管气相色谱法测定塑料食品包装材料中的DEHP[J].南京晓庄学院学报,2013,22(3):61–63.
[7]刘燕伟,周真巡,赵文峰,等.超声波萃取–HPLC检测饮料中DEHP的含量[J].食品研究与开发,2014(12):49–53.
[8]谈金辉,蒋永祥,孟靖颖.食品包装用塑料制品中六种邻苯二甲酸酯类化合物的测定方法研究[J].分析试验室,2007,26:133–135.
[9]庞世敏,袁敏,赵桂兰,等.气相色谱法测定邻苯二甲酸酯类增塑剂的研究[J].华南师范大学学报,2010,(4):70–74.
[10]王新豫,凌镇浩.开放式超声微波协同萃取测定PVC塑料中邻苯二甲酸酯类增塑剂研究[J].化学试剂,2009,31(2):109–111.
[11]马康,汤福寿,何雅娟,等.食品包装材料中13种增塑剂的毛细管气相色谱法测定[J].分析测试学报,2011,30(3):284–288.
[12]李波平,林勤保,宋欢,等.快速溶剂萃取–高效液相色谱测定塑料中邻苯二甲酸酯类化合物[J].应用化学,2008,25(1):63–66.
[13]张泽明,张洪海,李建龙,等.固相微萃取–气相色谱–质谱联用测定海水与沉积物中邻苯二甲酸酯类污染物[J].分析化学,2017,32(3):348–356.
[14]樊继彩,王姝婷,黄希汇,等.食用油中20种邻苯二甲酸酯的超高效液相色谱–质谱联用法测定[J].中国卫生检验杂志,2013(5):1 063–1 067.
[15]刘晓毅,蒋可心,石维妮,等.国内外食品接触材料中邻苯二甲酸酯类塑化剂迁移限量对比分析[J].食品工业科技,2011(10):397–399.
[16]张明明,刘玉兰,杨金强,等.油脂中邻苯二甲酸酯类塑化剂的吸附脱除研究[J].粮油食品科技,2015,23(5):32–36.