DHA甘油酯中增塑剂DBP含量的HPLC-MS/MS定性定量分析  

Qualitative and Quantitative Analysis of Plasticizer DBP Content in DHA Glyceride by HPLC-MS/MS

作　　者：谭新 陈迪 彭小雨 潘丽娜 李威 汪家琦 Tan Xin;Chen Di;Peng Xiaoyu;Pan Lina;Li Wei;Wang Jiaqi(Hu'nan Wanquan Yuxiang Biology Science and Technology Co.,Ltd.,Hu'nan,411300;Aoyou Dairy Industry(China)Co.,Ltd.,Hu'nan,410000)

机构地区：[1]湖南万全裕湘生物科技有限公司,湖南411300 [2]澳优乳业(中国)有限公司,湖南410000

出　　处：《当代化工研究》2023年第18期31-33,共3页Modern Chemical Research

基　　金：2023湖南长沙市科技计划重大专项“OPO结构油脂定向转化酶”(项目编号:kh2301009)。

摘　　要：本文建立了DHA甘油酯中增塑剂邻苯二甲酸二正丁酯(DBP)的反相高效液相色谱-质谱联用(RP-HPLC-MS/MS)定性定量分析方法。乙腈多次萃取DHA甘油酯原油并浓缩得到分析样品。色谱分离条件为:色谱柱为Shimadzu GIST C18(150mm×2.1mm,5μm),柱温为40℃,流动相为乙腈-水溶液,梯度洗脱,流速为0.3mL/min。质谱条件为:正离子多反应监测扫描(MRM)检测,外标法定量。该法灵敏度高,准确性好,其线性相关系数为0.9994,检测限为0.18μg/L,标准加标回收率在86.31%~114.08%之间,相对标准偏差(RSD)在1.70%~6.10%之间。分析发现引起DHA甘油酯产品DBP升高的原因主要是生产中塑料胶管和酯化酶中DBP的迁移,DHA甘油酯最终产品中DBP含量小于0.11mg/kg。In this study,a qualitative and quantitative analysis method for di-n-butyl phthalate(DBP)of plasticizer in DHA glycerides was established by reversed-phase high performance liquid chromatography-mass spectrometry(RP-HPLC-MS/MS).DHA glyceride crude oil was extracted and concentrated by acetonitrile for multiple times and then injected for analysis.The chromatographic separation conditions were Shimadzu GIST C18(150 mm×2.1 mm,5μm),column temperature was 40℃,mobile phase was acetonitrile-aqueous solution,gradient elution,flow rate was 0.3 mL/min.The mass spectrometry conditions were:positive ion multi-reaction monitoring scanning(MRM)detection,external standard quantification.The method has high sensitivity and good accuracy,its linear correlation coefficient is 0.9994,the detection limit is 0.18μg/L,the recovery rate of standard spike is between 86.31%~114.08%,and the relative standard deviation(RSD)is between 1.70%~6.10%.The analysis found that the migration of DBP from plastic hoses and esterases during the production process was the main reason for the increase of DBP in DHA glyceride products,and the DBP content in the final product of DHA glycerides was less than 0.11 mg/kg.

关 键 词：DHA甘油酯 DBP增塑剂 RP-HPLC-ESI-MS/MS 定性与定量分析 外标法 

分 类 号：O657[理学—分析化学] TQ225.24[理学—化学]