目的 采用核磁共振法測(cè)定甲磺酸阿帕替尼原料藥中甲磺酸阿帕替尼，提供一種有效的化學(xué)樣品測(cè)定手段。方法 以1，4-二硝基苯為內(nèi)標(biāo)，甲磺酸阿帕替尼為樣品，DMSO-d₆為溶劑，采用zg30脈沖序列在恒溫（25℃）下獲取¹H-NMR譜。以δ7.50處樣品定量峰和δ8.46處內(nèi)標(biāo)峰面積比值測(cè)定氫核磁共振譜，計(jì)算甲磺酸阿帕替尼的質(zhì)量分?jǐn)?shù)。并與質(zhì)量平衡法測(cè)定結(jié)果進(jìn)行了比較。結(jié)果 甲磺酸阿帕替尼在0.01～0.05 mmol/L線性關(guān)系良好。原料藥中甲磺酸阿帕替尼質(zhì)量分?jǐn)?shù)為96.66%，RSD值為0.33%。與質(zhì)量平衡法測(cè)定的結(jié)果96.25%基本一致。結(jié)論 本法樣品制備簡(jiǎn)單，測(cè)定快速，結(jié)果準(zhǔn)確，可用于測(cè)定甲磺酸阿帕替尼原料藥中甲磺酸阿帕替尼。

Objective To establish a nuclear magnetic resonance method to determine the content of apatinib mesylate in apatinib mesylate raw materials, so as to provide an effective method for chemical sample. Methods 1,4-Dinitrobenzene was used as an internal standard, apatinib mesylate was used as a sample, DMSO-d₆ was used as solvent, and the ¹H-NMR data of apatinib mesylate were determined at constant temperature (25℃) using zg30 pulse sequence. ¹H-NMR data of the sample peak area at δ7.50 and internal standard peak area ratio at δ8.46 were obtained. And the results of nuclear magnetic resonance method were compared with those of mass balance method. Results There was a good linear relationship of apatinib mesylate in the rang of 0.01-0.05 mmol/L. The content of apatinib mesylate in raw material was calculated to be 96.66% with RSD 0.33%. The result was consistent with that calculated by mass balance method (96.25%). Conclusion This method is simple, rapid, and accurate results, which can be used for determination content of apatinib mesylate in raw material.

國(guó)家重大新藥創(chuàng)制專項(xiàng)（2015ZX09303001）；中國(guó)食品藥品檢定研究院中青年基金資助項(xiàng)目（2014A6、2015A01）