GC-MS法测定奥美拉唑肠溶胶囊中17种邻苯二甲酸酯类

目的: 建立GC-MS法测定奥美拉唑肠溶胶囊中17种邻苯二甲酸酯类的含量,为奥美拉唑肠溶胶囊中邻苯二甲酸酯类增塑剂的质量控制提供有效的分析手段。 方法: 以甲醇为溶剂,采用超声提取及GC-MS方法。色谱柱:5%苯基,95%二甲基硅氧烷聚合物为固定相的石英毛细管柱(30 m×0.25 mm,0.25 μm);载气为高纯氦气;流速1.2 mL·min^-1;采用程序升温的方式;电离方式:电子轰击源(EI);电离能量:70 eV;离子源温度:230℃;监测方式:FS(定性),SIM(定量)。 结果: 8种邻苯二甲酸酯类在0.1~50 μg·mL^-1范围内呈线性关系,有9种邻苯二甲酸酯类在0.1~20 μg·mL^-1 范围内呈线性关系,r均大于0.99;在0.5~20μg· g^-1添加浓度范围内的平均回收率为74.8%~105.7%,RSD为2.5%~9.97%(n=6)。 结论: 本方法具有简便、准确、灵敏度高、专属性强的特点,可用于奥美拉唑肠溶胶囊中邻苯二甲酸酯类的检测。

Objective: To establish a GC-MS method for simultaneous determination of 17 kinds of phthalate esters in omeprazole enteric capsules and provide an effective analytical method for the quality control of phthalate esters in omeprazole enteric capsules. Methods: Phthalate esters were extracted with methanol as the solvent by ultrasonic. The contents of phthalate esters (PAEs) in omeprazole enteric capsules were determined by GC-MS method. The DB-5MS capillary column(30 m×0.25 mm,0.25 μm)was adopted with high-purity helium as the carrier gas with a flow rate of 1.2 mL·min^-1. Temperature-programmed method was used. Electronic ionization was performed with electron impaction source (EI),the electronic energy was 70 ev,the ion source temperature was 230℃,the scan models were full scan (qualitatively) and SIM (quantitatively). Results: There were linear relations in the range of 0.1-50 μg·mL^-1 for 8 phthalate esters,and 0.1-20 μg·mL^-1 for the other 9 phthalates esters,r ≥ 0.99,the average recovery within the added concentration range of 0.5-20 μg·g^-1 was 74.76-105.7% and RSD was 2.51-9.97% (n=6). Conclusion: The method is simple,accurate and reproducible,which can be applied in the determination of phthalate esters in omeprazole enteric capsules.