摘要
建立了牛奶中邻苯二甲酸二(2-甲氧基)乙酯(DMEP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-丁氧基)乙酯(DBEP)、邻苯二甲酸二戊酯(DPP)、邻苯二甲酸二(4-甲基-2-戊基)酯(BMPP)、邻苯二甲酸二己酯(DHXP)、邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)共9种邻苯二甲酸酯(PAEs)的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经正己烷提取后,用LC-Si固相萃取柱净化,以甲醇和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用HPLC-MS/MS电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,外标法定量。9种PAEs在2～200 ng/mL范围内均具有良好的线性关系,相关系数不低于0.9983,平均加标回收率为88.0%～103.1%,相对标准偏差均小于10%。该方法准确、灵敏、高效、环保,适用于牛奶中多种PAEs的同时测定。
A high performance liquid chromatography-tandem mass spectrophy（HPLC-MS/MS） was developed for determination of nine PAEs of bis（2-methoxyethyl） phthalate（DMEP）,diethyl phthalate（DEP）,benzyl butyl phthalate（BBP）,bis（2-n-butoxyethyl） phthalate（DBEP）,dipentyl phthalate（DPP）,bis（4-methyl-2-pentyl） phthalate（BMPP）,dihexyl phthalate（DHXP）,bis（2-ethyl-h exyl） phthalate（DEHP）,di-n-octyl phthalate（DNOP） residues in milk.The samples were extracted by n-hexane,and purified by LC-Si solid-phase extraction column.Methanol and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution.The analysis of target compounds was carried out by HPLC-MS/MS under positive electrospray ionization（ESI＋） and multiple reaction monitoring（MRM） mode.A external standard was used for quantitative analysis.The calibration curves were in good linearity between the peak area and the concentration of 2～200 ng/mL for nine PAEs with correlation coefficients not less than 0.9983.The average spiked recoveries for 9 PAEs were between 88.0% and 103.1% with relative standard deviations（RSDs） less than 10%.The proposed method is accurate,sensitive and high-efficient,and is applicable for simultaneous determination of PAEs in milk.
出处
《广东农业科学》
CAS
CSCD
北大核心
2012年第6期100-102,108,共4页
Guangdong Agricultural Sciences
关键词
高效液相色谱-串联质谱
牛奶
邻苯二甲酸酯
固相萃取
残留
high performance liquid chromatography-tandem mass spectrophy
milk
PAEs
solid phase extraction
residues
