UPLC-MS/MS法筛查口服液体药用复合膜中12种常见抗氧剂

目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)，用于筛查口服液体药用复合膜中12种常见抗氧剂。方法 采用正己烷为提取溶剂，回流2 h，提取目标化合物，用超高效液相色谱-串联质谱(UPLC-MS/MS)检测目标化合物含量;以Shim-pack GIST C18(100 mm×2.1 mm, 2 μm)为色谱柱，甲醇和水为流动相;质谱选用电喷雾(ESI)离子源，多反应监测(MRM)正离子模式进行定性定量分析。结果 12种抗氧剂在2~500 ng/mL的质量浓度范围内线性良好，相关系数r≥0.998 6，检测限为0.2~10.6 ng/g，回收率为78.9%~112.7%，相对标准偏差(RSD)为0.8%~7.0%(n=3);经检测，12批口服液体药用复合膜中均有抗氧剂检出，其中含量较高的有1010、1076和168。结论 该方法高效灵敏、准确可靠，可用于口服液体药用复合膜中12种常见抗氧剂的筛查。

Screening of 12 Common Antioxidants in Oral Liquid Medicinal Composite Films by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

The work aims to establish an ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method to screen 12 common antioxidants in oral liquid medicinal composite films. With n-hexane as the extraction solvent, the target compounds were extracted through a 2-hour reflux process. The content of the target compounds was then analyzed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Shim-pack GIST C18 (100 mm×2.1 mm, 2 μm) was employed as the chromatographic column and methanol and water were used as the mobile phase. Electrospray ionization (ESI) was utilized as the ion source, and multiple reaction monitoring (MRM) in positive ion mode was applied for qualitative and quantitative analysis. The 12 antioxidants exhibited good linearity within the concentration range of 2 to 500 ng/mL, with a correlation coefficient (r) ≥ 0.998 6. The detection limits ranged from 0.2 to 10.6 ng/g, and the recovery rates were between 78.9% and 112.7%. The relative standard deviation (RSD) ranged from 0.8% to 7.0% (n=3). Upon analysis, antioxidants were detected in all 12 batches of oral liquid medicinal composite films, with higher concentrations found in samples 1010, 1076, and 168. This method is highly efficient, sensitive, accurate, and reliable, making it suitable for the screening of 12 common antioxidants in oral liquid medicinal composite films.