加速溶剂萃取-高效液相色谱法检测瓦楞纸箱板中的多溴二苯醚
目的 建立一种加速溶剂萃取提取多溴二苯醚的高效液相色谱检测方法。方法 将多层瓦楞纸箱(板)剪至1 cm×1 cm大小, 取适量样品, 以乙醇-丙酮(1:1, V:V)为萃取溶剂, 加速溶剂萃取温度为150 ℃, 萃取压力为1500 psi, 静态萃取10 min, 重复萃取3次后, 用甲醇-水为流动相, 进行梯度洗脱, 226 nm波长进行检测。结果 对8种PBDEs的回收率在95%~105%之间, 精密度试验(n=6)的RSD0.999。结论 建立的方法与标准方法GB/Z 21276-2007检测结果无明显差异, 可以用于瓦楞纸箱(板)中的PBDEs检测。
Objective To establish a method for the determination of polybrominated diphenyl ethers (PBDEs) in corrugated box (cardboard) by high performance liquid chromatography (HPLC) with accelerated solvent extraction. Methods The corrugated box (cardboard) was cut to 1 cm×1 cm. The PBDEs were extracted with ethanol: acetone (1:1, V:V) as extraction solvent in 10 min with static extraction mode and repeated three times by accelerated solvent extraction (ASE) at 150 ℃ and pressure of 1500 psi. The extraction was analyzed by HPLC after using a gradient elution program of methanol-H2O as mobile phase, and detected at 226 nm. Results The recoveries of 8 PBDEs were 95%~105%, the relative standard deviations (RSDs) were under 3% (n=6), the limits of detection were 0.1~0.2 μg/mL, and the linear regression coefficients were above 0.9991. Conclusion The analysis results of PBDEs were satisfied by comparing with the standard method GB/Z 21276-2007. It can be used for the detection of PBDEs in the corrugated box (cardboard).
标题:加速溶剂萃取-高效液相色谱法检测瓦楞纸箱(板)中的多溴二苯醚
英文标题:Determination of polybrominated diphenyl ethers in corrugated box (cardboard) by accelerated solvent extraction-high performance liquid chromatography
作者:
李锦花 宁波出入境检验检疫局技术中心
李赛花 通标标准技术服务有限公司宁波分公司
许海峰 宁波出入境检验检疫局技术中心
陈丹超 宁波出入境检验检疫局技术中心
马明 宁波出入境检验检疫局技术中心
中文关键词:加速溶剂萃取,高效液相色谱,瓦楞纸箱(板),多溴二苯醚,
英文关键词:accelerated solvent extraction,high performance liquid chromatography,corrugated box (cardboard),polybrominated diphenyl ethers,
发表日期:2015-11-18
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