摘要
建立了一种快速、高效、灵敏的基质分散-磁性固相萃取/液相色谱（dMSPE/HPLC）方法,用于测定白酒中6种邻苯二甲酸酯类化合物（PAEs）残留量。样品用聚苯乙烯纳米磁性高分子材料进行富集处理后,经C8反相液相色谱柱（250 mm×4.6 mm×5μm）分离,以甲醇-水为流动相,梯度洗脱,230 nm检测。重点考察了样品p H值、吸附时间和洗脱剂的种类与用量等对PAEs富集回收率的影响。结果表明,在最佳实验条件下,6种PAEs在2-500 ng/L浓度范围内呈良好的线性关系,相关系数（r2）均不小于0.997 9;平均回收率为85.2%-101.2%,相对标准偏差（RSDs）为0.8%-9.2%;检出限（LODs）为0.22-4.5 ng/L,定量下限（LOQs）为1.2-10 ng/L。方法可用于白酒中PAEs的快速筛查和确证分析。
A rapid, sensitive and accurate method was developed for the simultaneous determination of 6 kinds of phthalic acid esters （PAEs） in wine samples by dispersive magnetic solid phase extraction coupled with high performance liquid chromatography（dMSPE/HPLC）. The wine samples were con- centrated with polystyrene nano-magnetie materials, then separated on a Cs analytical column （250 mm ×4.6 mm×5μm） using methanol - water as mobile phase by gradient elution, and detected at 230 nm via UV detector. The results showed that, under the optimal condition, good linearities for the target PAEs were obtained between 2 ng/L and 500 ng/L with correlation coefficients（ rE） not less than 0. 997 9. The spiked recoveries were between 85.2% and 101.2% with relative standard devia- tions （RSDs） of 0. 8% -9.2% . The limits of detection （LODs） were in the range of 0. 22 -4. 5 ng/ L and the limits of quantitation（LOQs） were 1.2 - 10 ng/L. The developed method could be applied in the routine analyses on PAEs in wine samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第11期1219-1223,共5页
Journal of Instrumental Analysis
基金
浙江省自然科学基金(LY14B04003)
宁波市自然科学基金(2014A610092)
国家级大学生创新创业训练计划项目(201313022007)
浙江省新苗计划项目(2013R401190)
关键词
白酒
邻苯二甲酸酯类化合物(PAEs)
聚苯乙烯磁性高分子材料
基质分散-磁性固相萃取
液相色谱
wine samples
phthalic acid esters（PAEs）
polystyrene nano-magnetic materials
dis-persive magnetic solid phase extraction（dMSPE）high performance liquid chromatography（HPLC）
