摘要
建立了同时测定水产品中24种邻苯二甲酸酯类化合物(PAEs)的气相色谱-质谱(GC-MS)分析方法。称取1.0 g样品于10 mL玻璃离心管中,加内标D4-DEHP溶液(10 mg/L)100μL,氯化钠0.5 g,以5 mL乙腈-乙酸乙酯(1∶1)超声提取5 min,4 000 r/min离心5 min,移取上层有机相。再加入3 mL乙腈-乙酸乙酯重复提取。合并两次的提取液浓缩至1～2 mL后,经Florisil玻璃固相萃取柱净化,洗脱液在50℃下氮吹至近干,用正己烷超声溶解定容至1 mL,供GC-MS分析。24种PAEs的定量下限(LOQ)为1～500μg/kg,检出限(LOD)为0.1～100μg/kg。选取鱼、虾为研究基质考察方法的准确度及精密度,24种PAEs在3个添加水平时的平均回收率及相对标准偏差(n=6)分别为73%～120%、2.0%～19.7%。结果表明,该方法提取效率高,净化效果好,重复性强,能够满足水产品中邻苯二甲酸酯类化合物的检测需求。
An internal standard quantitative method was developed for the simultaneous determination of 24 phthalate esters （PAEs） in sea foods by gas chromatography - mass spectrometry （ GC - MS）. 1.0 g Sample was taken into glass centrifuge tube, followed by adding 100 μL internal standard solu- tion（ 10 mg/L）, 0. 5 g NaCl and 5 mL acetonitrile - acetate ester（ 1 ： 1 ） extraction solution. The solution was mixed for 1 min, and extracted by ultrasonic for 5 min and centrifuged for 5 min at 4 000 r/min. The extraction step was repeated with 3 mL acetonitrile - acetate ester. The two extracted sol- vents were concentrated to 1 -2 mL, and then cleaned up through a glass Florisil SPE column. The analyses of 24 PAEs were carried out by GC - MS under selected ion monitoring （SIM） mode. The results showed that 24 PAEs had good linear relationships（ r 〉0. 999） between 0. 05 mg/L and 10.0 mg/L. The limits of quantitation（LOQs） of 24 PAEs were in the range of 1 - 500 μg/kg, and the limits of detection（LODs） were in the range of 0. 1 -100 μg/kg. The average recoveries of 24 PAEs in fish and prawn samples ranged from 73% to 120% , with relative standard deviations（ RSDs, n = 6） of 2.0% - 19.7% . The method was well suitable for the determination of PAEs in sea foods with its high sensitivity and precision.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第4期408-413,共6页
Journal of Instrumental Analysis
基金
国家科技支撑计划项目(2011BAK10B04)
关键词
水产品
邻苯二甲酸酯
固相萃取
气相色谱-质谱
sea foods
phthalate esters
SPE
gas chromatography -mass spectrometry（GC -MS）
