HPLC法测定灵芝孢子油中邻苯二甲酸酯类化合物  

Determination of Phthalic Acid Esters Compounds in Ganoderma Lucidum Spores Oil by HPLC

作　　者：金群杰 李晓颖 田克赞 毕研平 JIN Qun-jie;LI Xiao-ying;TIAN Ke-zan;BI Yan-ping(School of Pharmaceutical Sciences&Institute of Materia Medica,Shandong First Medical University&Shandong Academy of Medical Sciences,Taian 271000,China;Shandong Zhirentang Pharmaceutical Co.,Ltd.,Taian 271000,China)

机构地区：[1]山东第一医科大学药学院(药物研究所),山东泰安271000 [2]山东芝人堂药业有限公司,山东泰安271000

出　　处：《海峡药学》2024年第11期24-28,共5页Strait Pharmaceutical Journal

摘　　要：目的 建立固相萃取(Solid-Phase Extraction,SPE)净化结合HPLC分别测定灵芝孢子油中邻苯二甲酸二(2-乙基)己酯(DEHP)和邻苯二甲酸二正丁酯(DBP)含量的方法。方法 灵芝孢子油经甲醇萃取后使用SPE小柱净化,收集净化液经氮吹浓缩后,采用Supersil ODS_(2)色谱柱(250×4.6 mm,5μm),流动相为甲醇-水(检测DEHP流动相体积比为93∶7,检测DBP流动相体积比为75∶25),流速1.0 mL·min^(-1),柱温40℃,检测波长235 nm,外标法定量。结果 DEHP在0.11~44.52μg·mL^(-1)(r=0.9997)、DBP在0.11~44.28μg·mL^(-1)(r=0.9999)内呈良好的线性关系;DEHP和DBP的加样回收率分别为92.56%~97.55%和90.55%~97.70%。结论 建立的含量测定分析方法快速准确,灵敏度高,重复性和稳定性较好,适用于灵芝孢子油中DEHP和DBP的检测。OBJECTIVE A method for the determination of di(2-ethyl hexyl) phthalate(DEHP) and dibutyl phthalate(DBP) in Ganoderma lucidum spores oil by Solid Phase Extraction(SPE) and HPLC was established.METHODS Ganoderma lucidum spores oil was extracted with methanol and purified by SPE cartridge.The purified solution was concentrated by nitrogen blowing.The Supersil ODS_(2) column(250×4.6 mm,5 μm) was used.The mobile phase was methanol-water(detection DEHP mobile phase volume ratio was 93∶7,DBP mobile phase volume ratio was 75∶25),flow rate 1.0 mL·min~(-1),column temperature 40 ℃,detection wavelength 235 nm,external standard method.RESULTS The linear relationship of DEHP and DBP was good in the range of 0.11-44.52 μg·mL~(-1)(r=0.9997) and 0.11-44.28 μg·mL~(-1)(r=0.9999),respectively.The average recoveries were 92.56%-97.55% and 90.55%-97.70%,respectively.CONCLUSION The established analytical method is effective,accurate,highly sensitive,and reproducible and can be used for the individual determination of two plasticizers DEHP and DBP in Ganoderma Lucidum Spores Oil.

关 键 词：灵芝孢子油 邻苯二甲酸二(2-乙基)己酯 邻苯二甲酸二正丁酯 固相萃取 HPLC 

分 类 号：R927[医药卫生—药学]