高效液相色谱-三重四极杆/复合线性离子阱质谱法测定厄贝沙坦中的基因毒性杂质

阮瑜迪; 王春; 孟宪双; 叶琼; 马强; 程羽君

doi:10.13748/j.cnki.issn1007-7693.20232341

高效液相色谱-三重四极杆/复合线性离子阱质谱法测定厄贝沙坦中的基因毒性杂质

Determination of Genotoxic Impurities in Irbesartan by High Performance Liquid Chromatography-Triple Quadrupole/Composite Linear Ion Trap Mass Spectrometry

摘要

摘要:
目的建立抗高血压药厄贝沙坦中2-氰基-4’-溴甲基联苯和2-氰基-4’,4’-二溴甲基联苯2种基因毒性杂质的高效液相色谱-三重四极杆/复合线性离子阱质谱分析方法。
方法样品经溶剂溶解后，以Agilent Eclipse XDB-C₁₈(2.1 mm×100 mm，3.5 μm)色谱柱分离，梯度洗脱，洗脱液以多反应监测触发增强子离子扫描模式检测，采用二级质谱图进行定性，外标法定量。
结果 2种基因毒性杂质检出限和定量限分别为0.5和1.0 mg·kg⁻¹，在1~20 μg·L⁻¹内线性关系良好(R²>0.999)，在1、5、10 μg·L⁻¹ 3个加标浓度下，平均回收率为90%~110%，RSD<5%。
结论该方法操作简便，定性定量准确，能够满足厄贝沙坦中2种基因毒性杂质的分析需求。

Abstract:
OBJECTIVE To establish a high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry method of two genotoxic impurities, 2-cyano-4’-bromomethyl biphenyl and 2-cyano-4’,4’-bisbromomethyl biphenyl, in the antihypertensive drug irbesartan.
METHODS After solvent dissolution, the samples were separated by Agilent Eclipse XDB-C₁₈ column(2.1 mm×100 mm, 3.5 μm), eluted in gradient, and the eluate was detected by multiple reaction monitoring trigger enhancer ion scanning mode, qualitatively by second-level mass spectrometry and quantified by external standard.
RESULTS The detection and quantification limits of the two genotoxic impurities were 0.5 and 1.0 mg·kg⁻¹, respectively, with good linear relationship between 1−20 μg·L⁻¹(R²>0.999), at 1, 5 and 10 μg·L⁻¹, the average recovery was between 90% and 110%, and the RSD was <5%.
CONCLUSION The established method is easy to operate, accurate in qualitative and quantitative analysis, and can meet the analysis needs of the two genotoxic impurities in irbesartan.

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