邻苯二甲酸酯类首批化学对照品的标定及其色谱检测方法的建立

目的: 对供含量测定用的6种邻苯二甲酸酯类首批化学对照品进行标定,同时建立检测该类物质的色谱方法. 方法: 结合文献,应用UV、IR、NMR和ESI-MS等谱学技术对邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸二正戊酯(DAP)、邻苯二甲酸二异戊酯(DIAP)、邻苯二甲酸二环己酯(DCHP)和邻苯二甲酸二(2-甲氧乙基)酯(DMEP)6种邻苯二甲酸酯类化学对照品的结构进行鉴定,采用高效液相色谱法(HPLC)和气相色谱法(GC)进行纯度分析,利用质量平衡法进行定值;利用HPLC和GC同时检测多种邻苯二甲酸酯类化合物. 结果: HPLC法测得DMP、DBP、DAP、DIAP、DCHP、DMEP的纯度分别为99.4%、99.9%、99.5%、99.9%、99.9%、99.2%,GC法测得其纯度分别为99.6%、100.0%、99.4%、99.9%、100.0%、99.1%.在选定的HPLC色谱条件下,12种邻苯二甲酸酯类化合物的检测限为0.05~0.40 μg·mL^-1,定量限为0.20~1.20 μg·mL^-1,RSD为0.6%~0.9%;在选定的GC色谱条件下,其检测限为0.12~1.28 μg·mL^-1,定量限为0.47~4.28 μg·mL^-1,RSD为2.2%~2.7%. 结论: 建立了6种邻苯二甲酸酯类首批化学对照品;初步建立检测12种邻苯二甲酸酯类化学成分的HPLC和GC的方法,为该类化学成分的检测提供一定的参考依据.

Objective: To standardize the first batch of the reference standards of six phthalates and establish chromatograph analysis methods of phthalates. Methods: The structures of six phthalates(DMP, DBP, DAP, DIAP, DCHP, DMEP) were identified by UV, IR, NMR, and ESI-MS spectrometries.Their purities were determined by HPLC and GC methods.Eventually, their contents were determined by the mass balance method.Multiple kinds of phthalates were simultaneously determined by HPLC and GC. Results: The purity for DMP, DBP, DAP, DIAP, DCHP, and DMEP determined by HPLC was 99.4%, 99.9%, 99.5%, 99.9%, 99.9%, and 99.2%, and was 99.6%, 100.0%, 99.4%, 99.9%, 100.0%, and 99.1% by GC.Under the selected HPLC condition, the LOD of the 12 phthalates was 0.05-0.40 μg·mL^-1, LOQ was 0.20-1.20 μg·mL^-1, RSD was 0.6%-0.9%.Under the selected GC condition, the LOD was 0.12-1.28 μg·mL^-1, LOQ was 0.47-4.28 μg·mL^-1, RSD was 2.2%-2.7%. Conclusion: The establishment of the first batch of reference standards of six phthalates provides the material basis for the detection of such ingredients in food and cosmetics.Meanwhile, the HPLC and GC methods of simultaneously detecting 12 phthalates provide a reference for determination of such substances.