摘要
目的采用顶空气相色谱法,建立帕瑞昔布钠中甲醇、乙醇、二氯甲烷、正己烷和环己烷5种有机残留溶剂的测定方法。方法色谱柱为Agilent DB-624(30 m×0.32 mm,1.8μm)毛细管柱,采取程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为200℃,二甲基亚砜为溶剂,采用外标法计算残留溶剂的含量。结果在现定色谱条件下,甲醇、乙醇、二氯甲烷、正己烷和环己烷色谱峰均能达到有效分离,在考察的质量浓度内线性关系良好(r≥0.999 0),平均回收率为98.7%~100.8%(RSD<5%,n=9),定量限分别为0.51、0.43、0.50、0.29和0.08 mg·L-1。结论该法适用于帕瑞昔布钠原料药中5种有机残留溶剂的含量测定。
Objective To establish a capillary CJC method for the determination of residual solvents in parecoxib sodium by headspace sampling. Methods Agilent DB-624 capillary column （ 30 m×0.32 mm,1.8μm） was used on a programmed column temperature with FID detector. The temperature of the injection port was maintained at 200 ℃ and that of the detector at 250 ℃. The method was calculated by external standard method with DMSO as solvent. Results Linear responses were obtained for five residual solvents in their respective concentration ranges （ r ≥ 0. 999 0 ）. The concentration levels of average recoveries of methanol, ethanol, dichloromethane n-hexane and cyclohexane were 98.7 %-100. 8 % （RSD 〈 5 %, n = 9 ）, and the LOQ were 0. 51,0. 43,0. 50,0. 29,0. 08 mg. L-1, respectively. Conclusions The developed method is simple, sensitive, and accurate for the residual solvent analysis in raw material drug of parecoxib sodium.
出处
《沈阳药科大学学报》
CSCD
北大核心
2017年第10期889-892,928,共5页
Journal of Shenyang Pharmaceutical University
关键词
顶空气相色谱法
帕瑞昔布钠
残留溶剂
head-space capillary gas chromatography
parecoxib sodium
residual solvents
