| 高效液相色谱-串联质谱法同时测定牛奶中9种邻苯二甲酸酯 |
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| 引用本文： | 袁永添,刘正华,李拥军,李盛安,冯敏铃.高效液相色谱-串联质谱法同时测定牛奶中9种邻苯二甲酸酯[J].广东农业科学,2012,39(6):100-102,108. |
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| 作者姓名： | 袁永添 刘正华 李拥军 李盛安 冯敏铃 |
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| 作者单位： | 1. 中山市农产品质量监督检验所,广东中山,528403
2. 中山市小榄镇农业服务中心,广东中山,528415 |
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| 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。
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| 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 |
Simultaneous determination of nine Phthalic acid esters in milk by high performance liquid chromatography with tandem mass spectrometry |
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| YUAN Yong-tian
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LIU Zheng-hua
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LI Yong-jun
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LI Sheng-an
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FENG Min-ling.Simultaneous determination of nine Phthalic acid esters in milk by high performance liquid chromatography with tandem mass spectrometry[J].Guangdong Agricultural Sciences,2012,39(6):100-102,108. |
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| Authors: | YUAN Yong-tian LIU Zheng-hua LI Yong-jun LI Sheng-an FENG Min-ling |
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| Institution: | 1(1.Zhongshan Quality Supervision & Inspection Institute of Agricultural Products,Zhongshan 528403,China; 2.Agricultural Service Center of Xiaolan Town in zhangshan,Zhongshan 528415,China) |
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| Abstract: | 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. |
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| Keywords: | high performance liquid chromatography-tandem mass spectrophy milk PAEs solid phase extraction residues |
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