HPLC测定利奈唑胺原料药中3个降解杂质

Determination of Three Degradation Impurities in Linezolid Bulk Drug by HPLC

目的建立测定利奈唑胺原料药中3种主要降解杂质的高效液相色谱(HPLC)法。方法采用ZORBAX SB-C_(18)(4.6 mm×250 mm,5 μm)色谱柱,以0.1 %三氟乙酸乙腈溶液-0.1 %三氟乙酸水溶液为流动相,线性梯度洗脱,检测波长254 nm,流速1.0 ml/min,柱温30℃,进样量10 μl。结果利奈唑胺与杂质Ⅰ、杂质Ⅱ、杂质Ⅲ的线性范围分别为0.1072~10.72 μg/ml (r=1.0000),0.1026~10.26 μg/ml(r=0.9999),0.1033~10.33 μg/ml (r=0.9999),0.1015~10.15 μg/ml (r=0.9998);利奈唑胺与杂质Ⅰ、杂质Ⅱ、杂质Ⅲ的定量限分别为0.032,0.031,0.031,0.030 μg/ml;检测限分别为0.011,0.010,0.010,0.010 μg/ml;3种杂质平均回收率分别为97.36 %,96.76 %和95.54 %,RSD分别为1.62%,1.22%和1.82%。结论该方法简便灵敏,结果准确可靠,重复性好,可用于利奈唑胺有关物质的控制。

Objective To establish an HPLC method for the assay of three degradation impurities in linezolid bulk drug.Methods A ZORBAX SB-C_(18)(4.6 mm×250 mm, 5 μm) column was used,using 0.1 % trifluoroacetic acid acetonitrile solution-0.1 % trifluoroacetic acid aqueous solution as mobile phase of linear gradient elution.The detection wavelength was set at 254 nm.The flow rate was 1.0 ml/min and the column temperature was 30 ℃.The injection volume was 10 μl. Results The calibration curves of linezolid,impurity Ⅰ,Ⅱ and Ⅲ showed good linearities in the range of 0.1072-10.72 μg/ml(r=1.0000),0.1026-10.26 μg/ml(r=0.9999),0.1033-10.33 μg/ml(r=0.9999) and0.1015-10.15 μg/ml(r=0.9998),respectively.The LOQs for linezolid,impurity Ⅰ,Ⅱ and Ⅲ were 0.032,0.031,0.031 and 0.030 μg/ml,respectively;LODs were 0.011,0.010,0.010 and 0.010 μg/ml,respectively. The average recoveries for three degradation impurities were 97.36 %, 96.76 % and 95.54 %, with RSDs of 1.62 %, 1.22 % and1.82%. Conclusion The method is simple,sensitive,accurate and reproducible,and can be used for control of related substance in linezolid bulk drug.