Determination of related impurities in trazodone hydrochloride API by HPLC-MS/MS
奉艳花 1邓鸣1
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作者信息
1. 广西壮族自治区药品检验研究院,南宁 530021
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摘要
目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定盐酸曲唑酮中相关杂质的含量.方法:采用 Agilent ZORBAX Eclipse Plus C18 色谱柱(2.1 mm × 100 mm,1.8 µm),以 0.1％甲酸溶液-乙腈为流动相,梯度洗脱,流速0.2 mL·min-1,柱温30 ℃,采用电喷雾离子化源(ESI),多反应检测(MRM)模式,正离子模式扫描.结果:测定了盐酸曲唑酮原料药中的5个相关杂质,分别为三唑并吡啶酮、曲唑酮-N-氧化物、脱氯曲唑酮、4-乙基曲唑酮、曲唑酮异丁醚类似物,杂质在测定的质量浓度范围内线性关系良好,r均≥0.999 5;平均回收率为91.9％～99.4％,RSD≤3.9％;测定的3批原料药中均检出了曲唑酮N-氧化物和脱氯曲唑酮,其中2批还检测到极微量的4-乙基曲唑酮.结论:建立的方法可测定盐酸曲唑酮原料药中的5种相关杂质,能更有效的评估和控制其质量.
Abstract
Objective:To establish an HPLC-MS/MS method for the determination of related impurities in traz-odone hydrochloride API.Methods:The impurities were separated on an Agilent ZORBAX Eclipse Plus C18column(2.1 mm x 100 mm,1.8 μm)using a gradient elution of 0.1％formic acid solution and acetonitrile at a flow rate of 0.2 mL·min-1 at column temperature of 30 ℃,and determined by electrospray ionization source(ESI)com-bined with multiple reaction detection(MRM)in the positive ion mode.Results:The related impurities(triazol-opyridone,trazodone N-oxide,dechlorinated trazodone,4-ethyltrazodone,and trazodone isobutyl ether analogue)in trazodone hydrochloride API were determined.The linear relationship of five impurities was good in correspond-ing concentration ranges with correlation coefficients(r)of more than 0.999 5.The average recoveries varied be-tween 91.9％and 99.4％with RSD ≤3.9％.Trazodone N-oxide and dechlorinated trazodone were detected in all three batches,and extremely trace amounts of 4-ethyltrazodone were detected in two batches.Conclusion:The es-tablished method can determine the content of five related impurities in trazodone hydrochloride API,and can more effectively evaluate and control the quality of trazodone hydrochloride API.
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