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目的建立UPLC-MS测定薄膜衣片中16种邻苯二甲酸酯类塑化剂含量的方法。方法采用甲醇提取,Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)同时串联Waters PFCs Isolator捕集柱(2.1 mm×50 mm),以0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,流速:0.4 mL·min~(-1);采用电喷雾离子源,正离子模式,多反应监测模式检测。结果在实验条件下,16种塑化剂分离良好;DBP、DIBP检测限为0.5 mg·kg~(-1),其余14种塑化剂检测限为0.1 mg·kg~(-1);DBP、DIBP在0.20~1.00μg·mL~(-1)内,其余14种塑化剂在0.05~1.00μg·mL~(-1)内,峰面积与检测浓度之间的线性关系良好(r≥0.995);平均回收率均在83%~115%之间。结论该方法操作简单、快速、准确,适用于薄膜衣片中邻苯二甲酸酯类塑化剂的测定。
OBJECTIVE To establish a method for the determination of 16 phthalate plasticizers in film-coated tablets by UPLC-MS. Methods A Waters ACQUITY UPLC BEH C 18 column (2.1 mm × 50 mm, 1.7 μm) was used in this study. A series of Waters PFCs Isolator trapping columns (2.1 mm × 50 mm) were connected in series with 0.1% formic acid in water and methanol Phase and gradient elution. The flow rate was 0.4 mL · min ~ (-1). Electrospray ionization (ESI) ion source, positive ion mode and multi-reaction monitoring mode were used. Results Under the experimental conditions, 16 kinds of plasticizers were well separated. The detection limit of DBP and DIBP was 0.5 mg · kg -1 and the limit of detection of the other 14 plasticizers was 0.1 mg · kg -1. DBP , DIBP was 0.20-1.00 μg · mL -1, while the other 14 kinds of plasticizers were in the range of 0.05-1.00 μg · mL -1. The linear relationship between peak area and test concentration was good (r ≥ 0.995). The average recoveries ranged from 83% to 115%. Conclusion The method is simple, rapid and accurate and is suitable for the determination of phthalate plasticizers in film-coated tablets.