UPLC-MS测定薄膜衣片中16种邻苯二甲酸酯类塑化剂

Determination of 16 Kinds of Phthalates in Film-coated Tablets by UPLC-MS

关键词:  超高效液相色谱-串联质谱法  邻苯二甲酸酯类化合物  薄膜衣片  塑化剂

Key words:  UPLC-MS  phthalates (PAEs)  film-coated tablet  plasticizer

摘要:

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 C₁₈色谱柱（2.1 mm×50 mm，1.7 μm）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0.20~1.00 μg·mL^-1内，其余14种塑化剂在0.05~1.00 μg·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。

Abstract:

OBJECTIVE To establish an UPLC-MS method for simultaneous determination of 16 kinds of phthalates in film-coated tablets. METHODS Phthalates were extracted with methanol. Separation was performed on Waters ACQUITY UPLC BEH C₁₈ column (2.1 mm×50 mm, 1.7 μm) connected in series with Waters PFCs Isolator column (2.1 mm×50 mm). 0.1% formic acid solution and methanol were used as mobile phases in gradient elution, flow rate was 0.4 mL·min^-1. ESI⁺ and multi-reaction monitoring (MRM) were adopted in MS/MS. RESULTS Sixteen kinds of phthalates could be completely separated. The detection limits of DBP and DIBP were 0.5 mg·kg^-1, and other 14 kinds of phthalates were 0.1 mg·kg^-1. DBP and DIBP in the range of 0.20-1.00 μg·mL^-1, and other 14 kinds of phthalates in the range of 0.05-1.00 μg·mL^-1 had good linear relationships with relative coefficients (r ≥ 0.995). The average recoveries were from 83% to 115%. CONCLUSION The method is simple, rapid and accurate, and can be applied to simultaneous determination of phthalates in film-coated tablets.