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

Determination of polybrominated diphenyl ethers in corrugated box(cardboard) by accelerated solvent extraction-high performance liquid chromatography

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RSD〈3%,检测限为0.1~0.2μg/m L,线性回归系数〉0.999。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 crux 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 ~C and pressure of 1500 psi. The extraction was analyzed by HPLC after using a gradient elution program of methanol-H20 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 Ixg/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）.