HPLC法测定吡嗪酰胺的含量及有关物质
Determination of pyrazinamide and its related substances by HPLC
-
摘要: 建立用于吡嗪酰胺含量及其有关物质测定的HPLC法，为吡嗪酰胺原料药制定质量控制标准，并采用LCMS-IT-TOF对检出主要杂质的结构进行推定。色谱柱为TSK-gel ODS-100V(250 mm×4.6 mm，5 μm)，流动相为甲醇-水(冰醋酸调节pH 3.0)(8∶92)，检测波长为268 nm，柱温为35 ℃，流速为1.0 mL/min。对方法进行了系统的验证:主峰能与相邻杂质峰较好地分离；在0.4~250 μg/mL范围内，吡嗪酰胺的质量浓度与峰面积呈良好的线性关系(r=1.00)；最低检测限和最低定量限分别为6.5和40.5 ng/mL；9批样品含量测定结果与英国药典的非水电位滴定法结果一致。所建方法专属、耐用，操作简便，可用于吡嗪酰胺原料的含量及有关物质测定。已建议中国药典和国际药典收载。
-
关键词:
- 吡嗪酰胺 /
- 高效液相色谱法 /
- LCMS-IT-TOF /
- 含量测定 /
- 有关物质
Abstract: An HPLC method was established for the determination of pyrazinamide and its related substances. The method was carried out on a TSK-gel ODS-gel C18 column(250 mm×4. 6 mm, 5 μm)with a mobile phase consisting of methanol-water(pH 3. 0 adjusted with glacial acetic acid)(8 ∶92)at the flow rate of 1. 0 mL/min. The detection wavelength was set at 268 nm and the column temperature was kept at 35 °C. There was fair resolution between pyrazinamide and its related substance. The calibration curves were linear over the range of 0. 4 μg/mL and 250 μg/mL(r=1. 00). The limits of detection and quantitation were 6. 5 ng/mL and 40. 5 ng/mL, respectively. The contents data of nine batches of pyrazinamide determined by the developed method were consistent with those measured by non-aqueous potentiometric titration(BP 2012). The established HPLC method is specific, accurate, durable and easy to operate, has been proposed to be used in the Chinese Pharmacopoeia and the International Pharmacopoeia. It could be applied for the determination of pyrazinamide and its related substances.-
Keywords:
- pyrazinamide /
- HPLC /
- LCMS-IT-TOF /
- determination of content /
- related substances
-
-
[1] Zou Q,Zheng YY,Li BD.Synthesis of pyrazinamide[J].Jiangsu Chem Ind(江苏化工),2005,6(33)Suppliment:124-126. [2] Zhai J.Synthesis of 2-Cyanopyrazine[D]. Hangzhou: Zhejiang University,2003. [3] Liu JH,Cheng YB,Li XL.Determiantion of pyrazinamide tablets by RP-HPLC[J].Jiangsu Pharm Clin Res(江苏药学与临床研究),1999,7(3):17-18. [4] Pang QY,Lu Y,Yu L.Analytical separation of rifampicin,isoniazid and pyrazinamide in compound rifampicin tablets by RP-HPLC[J].J Pharm Anal(药物分析杂志),1998,18(4):259-261. [5] Li QL,Jiang XM,Shi CY.Determination of rifampicin,isoniazid and pyrazinamide in compound rifamipicin tablet by HPLC[J].Chin J Antibiot(中国抗生素杂志),2002,27(9):570-571. [6] Li LX,Ao SC,Duan XY.Determination of pyrazinamide by HPLC[J].Chin J Hosp Pharm(中国医院药学杂志),2002,5(22):317. [7] Yan XM,Ye Y.Determination of isoniazid,rifampicin and pyrazinamide in blood serum by HPLC[J].Jiangxi Med(江西医药),2008,43(11):1 231-1 233. [8] Cai ZY,Zhou BH,Li JY.Determination the content of isoniazid and pyrazinamide in tablets by ion-pair-RP-HPLC[J].Chin Pharm(中国药师),2005,8(7):562-563.
计量
- 文章访问数: 1083
- HTML全文浏览量: 0
- PDF下载量: 1553
下载:
