| 引用本文: | 杨梅,廉向金,张亿.UPLC-MS测定薄膜衣片中16种邻苯二甲酸酯类塑化剂[J].中国现代应用药学,2017,34(10):1437-1440. |
| YANG Mei,LIAN Xiangjin,ZHANG Yi.Determination of 16 Kinds of Phthalates in Film-coated Tablets by UPLC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(10):1437-1440. |
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| 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。 |
| 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 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.10.016 |
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| Determination of 16 Kinds of Phthalates in Film-coated Tablets by UPLC-MS |
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YANG Mei, LIAN Xiangjin, ZHANG Yi
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Chengdu Institute of Food and Drug Control, Chengdu 610045, China
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| 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. |
| Key words: UPLC-MS phthalates (PAEs) film-coated tablet plasticizer |
