UPLC–MS–MS法测定塑料包装材料中四溴双酚A
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摘要
建立超高效液相色谱–串联质谱法(UPLC–MS–MS)测定塑料包装材料中四溴双酚A的含量。塑料包装材料样品经研磨粉碎后,采用纯甲醇进行超声萃取,萃取液经氮吹浓缩后用UPLC–MS–MS测定。四溴双酚A的质量浓度在2.5~50 ng/g范围内与色谱峰面积呈良好的线性关系,线性相关系数为0.999 8,检出限为0.6μg/kg,定量限为2.0μg/kg。加标平均回收率为93.2%~97.3%,测定结果的相对标准偏差为1.0%~2.6%(n=6)。该方法简便、快速、准确度高,可为塑料包装材料产品质量监测提供检测方法。
The method for determination of tetrabromobisphenol A in plastic packaging materials by ultra performance liquid chromatography–tandem mass spectrometry(UPLC–MS–MS) was established. The samples of plastic packaging material were grinded and crushed,and then were sonicated by the pure methanol,and were concentrated by nitrogen and were determined by UPLC–MS–MS. The content of tetrabromobisphenol A had good linear relations with chromatographic peak area in the range of 2.5–50 ng/g,and the correlation coefficient was 0.999 8, the detection limit was 0.6 μg/kg,the limit of quantification was 2.0 μg/kg. The average recoveries were 93.2%–97.3%,and the relative standard deviation of determination results was 1.0%–2.6%(n=6). The method is simple,rapid and accurate, it can provide a test method for the quality monitoring of plastic packaging materials.
The method for determination of tetrabromobisphenol A in plastic packaging materials by ultra performance liquid chromatography–tandem mass spectrometry(UPLC–MS–MS) was established. The samples of plastic packaging material were grinded and crushed,and then were sonicated by the pure methanol,and were concentrated by nitrogen and were determined by UPLC–MS–MS. The content of tetrabromobisphenol A had good linear relations with chromatographic peak area in the range of 2.5–50 ng/g,and the correlation coefficient was 0.999 8, the detection limit was 0.6 μg/kg,the limit of quantification was 2.0 μg/kg. The average recoveries were 93.2%–97.3%,and the relative standard deviation of determination results was 1.0%–2.6%(n=6). The method is simple,rapid and accurate, it can provide a test method for the quality monitoring of plastic packaging materials.
引文
[1]李锋丽.水体和土壤环境中四溴双酚A的分析方法[D].济南:山东大学,2012.
[2]HOFFMANN M,FIEDOR E,PTAK A.Bisphenol A and its derivatives tetrabromobisphenol A and tetrachlorobisphenol A induce apelin expression and secretion in ovarian cancer cells through a peroxisome proliferator-activated receptor gammadependent mechanism[J].Toxicology letters,2017,269(5):15–22.
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[6]YUAN J P,CUI Z J,CHENG C G,et al.Rapid and simultaneous determination of tetrabromobisphenol A and hexabromocyclododecane diastereoisomers in soil by matrix solidphase dispersion with bamboo charcoal as dispersive adsorbent[J].Acta chromatographica,2017,29(1):1–6.
[7]谢宇奇,欧阳辉祥,黄勇富,等.藏红T褪色光度法测定四溴双酚A的含量[J].光谱实验室,2013,30(6):3 366–3 371.
[8]邱丰艳,韩飞,郑增尧,等.丹酰氯柱前衍生–HPLC荧光法测定食品接触材料中烷基酚类化合物迁移量[J].分析试验室,2017,36(10):1 188–1 192.
[9]李彬,刘丽,陈麒宇,等.微波辅助萃取–衍生气相色谱–电子捕获检测器法测定电子电气产品中的四溴双酚A[J].分析试验室,2010,29(1):64–67.
[10]王云玉,许志钦,李丹,等.GC–MS法测定涂料中的四溴双酚A[J].分析测试学报,2014,33(6):724–727.
[11]章勇,张蓓蓓,穆肃,等.液质联用法测定水中六溴环十二烷和四溴双酚A[J].环境科学与技术,2014,37(4):107–112.
[12]LI J,CHEN T,WANG Y,et al.Simple and fast analysis of tetrabromobisphenol A,hexabromocyclododecane isomers,and polybrominated diphenyl ethers in serum using solid-phase extraction or Qu ECh ERS extraction followed by tandem mass spectrometry coupled to HPLC and GC[J].Journal of separation science,2016,40(3):709–716.
[13]李志刚.液相色谱串联质谱测定纺织品中的四溴双酚A[J].分析测试学报,2017,36(10):1 260–1 264.
[14]丁洁,张圣虎,刘济宁,等.液相色谱–串联质谱法测定污水处理厂水样中双酚A、四溴双酚A及烷基酚类化合物[J].色谱,2014,32(5):529–534.
[15]张圣虎,张易曦,吉贵祥,等.高效液相色谱–串联质谱法测定儿童和成人尿液中双酚A、四溴双酚A和辛基酚[J].分析化学,2016,44(1):19–24.
[2]HOFFMANN M,FIEDOR E,PTAK A.Bisphenol A and its derivatives tetrabromobisphenol A and tetrachlorobisphenol A induce apelin expression and secretion in ovarian cancer cells through a peroxisome proliferator-activated receptor gammadependent mechanism[J].Toxicology letters,2017,269(5):15–22.
[3]高丹丹,于云江,王琼,等.不同暴露方式四溴双酚A的代谢及毒性特征[J].环境与健康杂志,2015,32(2):165–168.
[4]孙丰超,杨苏文,徐范范,等.四溴双酚A的鱼类毒性效应及其机制研究进展[J].环境与健康杂志,2013,30(2):178–181.
[5]李玲玲,刘世诚,朱崇岭,等.河道底泥中四溴双酚A厌氧降解及代谢途径[J].环境化学,2014,33(5):837–843.
[6]YUAN J P,CUI Z J,CHENG C G,et al.Rapid and simultaneous determination of tetrabromobisphenol A and hexabromocyclododecane diastereoisomers in soil by matrix solidphase dispersion with bamboo charcoal as dispersive adsorbent[J].Acta chromatographica,2017,29(1):1–6.
[7]谢宇奇,欧阳辉祥,黄勇富,等.藏红T褪色光度法测定四溴双酚A的含量[J].光谱实验室,2013,30(6):3 366–3 371.
[8]邱丰艳,韩飞,郑增尧,等.丹酰氯柱前衍生–HPLC荧光法测定食品接触材料中烷基酚类化合物迁移量[J].分析试验室,2017,36(10):1 188–1 192.
[9]李彬,刘丽,陈麒宇,等.微波辅助萃取–衍生气相色谱–电子捕获检测器法测定电子电气产品中的四溴双酚A[J].分析试验室,2010,29(1):64–67.
[10]王云玉,许志钦,李丹,等.GC–MS法测定涂料中的四溴双酚A[J].分析测试学报,2014,33(6):724–727.
[11]章勇,张蓓蓓,穆肃,等.液质联用法测定水中六溴环十二烷和四溴双酚A[J].环境科学与技术,2014,37(4):107–112.
[12]LI J,CHEN T,WANG Y,et al.Simple and fast analysis of tetrabromobisphenol A,hexabromocyclododecane isomers,and polybrominated diphenyl ethers in serum using solid-phase extraction or Qu ECh ERS extraction followed by tandem mass spectrometry coupled to HPLC and GC[J].Journal of separation science,2016,40(3):709–716.
[13]李志刚.液相色谱串联质谱测定纺织品中的四溴双酚A[J].分析测试学报,2017,36(10):1 260–1 264.
[14]丁洁,张圣虎,刘济宁,等.液相色谱–串联质谱法测定污水处理厂水样中双酚A、四溴双酚A及烷基酚类化合物[J].色谱,2014,32(5):529–534.
[15]张圣虎,张易曦,吉贵祥,等.高效液相色谱–串联质谱法测定儿童和成人尿液中双酚A、四溴双酚A和辛基酚[J].分析化学,2016,44(1):19–24.