摘要
目的建立硅胶／N-丙基乙二胺（PSA）混合固相萃取结合气相色谱-质谱联用测定食用植物油中17种邻苯二甲酸酯类化合物（PAE）的方法，并对杭州超市采集的25份塑料桶装食用油的PAEs含量进行评估。方法样品食用植物油加入D4-邻苯二甲酸二（2-乙基）己酯（D4-DEHP）内标应用液，用乙腈提取，旋涡混匀1min，3050xg离心5min，取上层乙腈相用硅胶／PSA混合固相萃取柱净化，乙腈洗脱，洗脱液在50℃下用氮吹仪吹干，加正己烷定容至1．0ml，然后用气相色谱质谱测定17种PAE，采用内标法定量，并对方法的检测限、精密度和准确度进行评价。检测了从杭州超市采集的25份塑料桶装食用油的PAE含量。结果采用Dd-DEHP内标法，17种PAE在对应的浓度范围内线性较好，相关系数为0．994～1．000，最低检测浓度为0．05—0．15ug／ml，17种PAE加标回收率为78．3％～108．9％，RSD为4．3％～12．1％（n=6），方法检出限为0．1～0．2mg／kg。杭州市售的25份塑料桶装食用植物油中检出邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-乙基）己酯（DEHP），检出率分别为12％（3／25）、24％（6／25）、100％（25／25）、96％（24／25）、100％（25／25），含量范围为〈0．1～1．8mg／kg，其他12种PAE均未检出；DBP含量范围为〈0．1—1．3mg／kg，16％（4／25）超过国家规定的迁移限量值（0．3mg／kg），DEHP含量范围为0．2～1．8mg／kg，12％（3／25）超过国家规定的迁移限量值（1．5mg／kg）。结论建立的硅胶／PSA混合固相萃取结合气相色谱．质谱联用方法可以满足食用植物油中PAE检测要求；杭州市场采集的25份塑料桶装食用油中检出了DMP、DIBP、DEP、DBP、DEHP等PAE组分。
Objective We aimed to establish a quantified method for the 17 phthalate acid esters （PAE） in edible vegetable oil by gas chromatography-mass spectrometry （GC-MS） with the pretreatment of acetonitrile extraction and silica/N-（n-propyl） ethylenediamine （silica/PSA） mixed solid phase extraction column and evaluated the PAE of 25 edible oil samples from supermarkets in Hangzhou city. Methods The internal standard solution （D4-DEHP） was added in edible vegetable oil sample. The analytes were extracted by acetonitrile with 1 min vortex, and centrifuged at 3050 x g for 5 min. The supernatant was then cleaned with silica/PSA column, and eluted with acetonitrile. The elution was dried with N2 flow at 50 ℃ and diluted to 1.0 ml with hexane. Then, 17 PAE were tested by GC-MS and quantified with internal standards. The repeatability and sensitivity of the assay were evaluated. PAE were then determined in 25 plastic buckets of edible vegetable oil from supermarkets in Hangzhou cityl Results By the quantification of internal standard of D4-DEHP, a good linearity range of related 17 PAE was observed. The correlation coefficient was 0. 994 - 1. 000 and the standard lowest quantified level was 0. 05 -0. 15 ug/ml. The spiking recoveries of 17 PAE were 78. 3% - 108.9 % with the RSD of 4. 3% - 12. 1% （n =6）. The method detection limits were 0. 1 -0. 2 mg/kg. In 25 plastic buckets of edible vegetable oil from Hangzhou, DMP, DEP, DIBP, DBP and DEHP were detected at the range of 〈 0. 1 - 1.8 mg/kg and the detection rates were 12% （ 3/25 ）, 24% （6/25）, 100% （25/25）, 96% （24/25） and 100% （25/25）, respectively. Other 12 PAE was not detected. For DBP with the level of 〈0. 1 to 1.3 mg/kg, the results of 16% （4/25） samples exceeded the regular migrating limit of 0. 3 mg/kg. For DEHP of 〈0. 2 - 1.8 mg/kg, the data of 12% （3/25） samples were beyond the regular migrating limit of 1.5 mg/kg. Conclusion The pretreatment by silica/PSA mixed solid phase extraction column can satisfy the P
出处
《中华预防医学杂志》
CAS
CSCD
北大核心
2012年第6期561-566,共6页
Chinese Journal of Preventive Medicine
