三峡库区调味油脂产品中邻苯二甲酸酯类塑化剂的含量测定和分析

Determination and analysis of phthalate plasticizer content in flavoring oil products in three gorges reservoir area

中文关键词:  气相色谱-三重四极杆串联质谱法  三峡库区  调味油脂  邻苯二甲酸二正丁酯  邻苯二甲酸二(2-乙基)己酯

英文关键词:gas chromatography-triple quadrupole tandem mass spectrometry  three gorges reservoir area  flavoring oil  dibutyl phthalate  bis (2-ethylhexyl) phthalate

中文摘要:

      目的 采用气相色谱-三重四极杆串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry, GC-MS/MS)测定三峡库区调味油脂产品中的邻苯二甲酸二正丁酯(dibutyl phthalate, DBP)、邻苯二甲酸二(2-乙基)己酯[bis(2-ethylhexyl) phthalate, DEHP] 2种塑化剂的含量, 并对污染情况进行分析。方法 样品采用乙腈提取, 固相萃取(solid-phase extraction, SPE)玻璃小柱净化, 氮吹近干后正己烷复溶, 经气相色谱-三重四极杆串联质谱法测定。结果 DBP、DEHP在一定浓度范围内线性关系良好, 相关系数均大于0.998, 检出限分别为0.05、0.10 mg/kg, 定量限分别为0.17、0.33 mg/kg, 平均加标回收率为82.79%~96.70%, 相对标准偏差为0.59%~1.76%。在采集的32组调味油脂样品中, DBP的检出率高达68.75%, 含量范围在0.15~517.00 mg/kg; DEHP检出率为28.12%, 含量范围在0.57~125.00 mg/kg, 超标率分别为62.50%和-18.75%。结论 三峡库区调味油脂产品中存在一定程度的邻苯二甲酸酯类物质污染, 可能与生产、环境等方面的迁移污染相关, 需引起重视并进行连续监测。

英文摘要:

      Objective To determine the content of dibutyl phthalate (DBP) and bis(2-ethylhexyl) phthalate (DEHP) plasticizers in flavoring oils and oils from the three gorges reservoir area by gas chromatography- triple quadrupole tandem mass spectrometry (GC-MS/MS), and analyze the pollution situation. Methods The samples were extracted by acetonitrile, purified by solid phase extraction (SPE) with glass column, redissolved by n-hexane after nitrogen blowing-drying, and determined by gas chromatography-triple quadrupole tandem mass spectrometry. Results DBP and DEHP had a good linear relationship in a certain concentration range, the correlation coefficients were both greater than 0.998, the limits of detection were 0.05 and 0.10 mg/kg, and the limits of quantification were 0.17 and 0.33 mg/kg, respectively. The average recovery rates were 82.79%?96.70%, and the relative standard deviations were 0.59%?1.76%. In 32 groups of flavoring oil samples, the detection rate of DBP was as high as 68.75%, and the content ranged from 0.15 mg/kg to 517.00 mg/kg. The detection rate of DEHP was 28.12%, the content ranged from 0.57 to 125.00 mg/kg. The over-standard rates were 62.50% and ?18.75%, respectively. Conclusion There is a certain degree of phthalate ester pollution in the flavoring oil products in the three gorges reservoir area, which may be related to the migration in production and environment, so we should pay attention to and continuously monitored.