摘要
目的:建立药用卤化丁基胶塞中17种抗氧剂向注射用伏立康唑中迁移的检测方法。方法:采用InertSustain C18色谱柱(4.6 mm×250 mm,5μm),以0.02 mol·L^-1甲酸铵(甲酸调节pH至5.0)-甲醇为流动相,梯度洗脱,流速1.0 mL·min^-1,检测波长277 nm,柱温30℃,进样量10μL。结果:17种抗氧剂之间的分离度良好;抗氧剂1076、1010、1035、168、1520在1~16μg·m L^-1浓度范围内线性关系良好(r2=0.9999);其余抗氧剂在0.5~8.0μg·mL^-1浓度范围内线性关系良好(r2=0.9999)。方法精密度、重复性、回收率、稳定性均符合有关规定。4家企业12批次样品中共计检出10种抗氧剂发生迁移,分别为DBHQ、BHT-COOH、BHT-OH、BHT-CHO、DBP、BHT-Q、BHT、2246、1035、445。结论:该方法灵敏度高,操作简单,重复性好,可用于药用卤化丁基胶塞中17种抗氧剂向注射用伏立康唑中迁移量的测定。
Objective:To establish an HPLC method for monitoring the migration of 17 antioxidants from pharmaceutical halogenated butyl rubber stopper to voriconazole for injection. Methods:HPLC was performed on an InertSustain C18 column(4.6 mm×250 mm,5 μm)with the mobile phase of 0.02 mol·L^-1 ammonium formate(adjusted to pH 5.0 with formic acid)-methanol(gradient elution). The flow rate was 1.0 mL·min^-1,the detection wavelength was 277 nm,the column temperature was maintained at 30 ℃ and the sample volume was 10 μL. Results:The resolutions between 17 antioxidants were great. The antioxidants(1076,1010,1035,168,1520) and the other antioxidants showed good linear relationship in the concentration range of 1-16 μg·mL^-1(r2=0.999 9)and 0.5-8.0 μg·m L^-1(r2=0.999 9),respectively. The precision,repeatability,recovery rate and stability were in line with the relevant requirements. A total of 10 kinds of antioxidants were detected in 12 batches of samples from 4 companies,which were DBHQ,BHT-COOH,BHT-OH,BHT-CHO,DBP,BHT-Q,BHT,2246,1035,445. Conclusions:The method is sensitive,rapid and accurate with good repeatability,which is used to determine the migration of 17 antioxidants from pharmaceutical halogenated butyl rubber stopper to voriconazole for injection.
作者
张旭
傅萍
谢华
袁军
常艳波
ZHANG Xu;FU Ping;XIE Hua;YUAN Jun;CHANG Yan-bo(Sichuan Institute for Food and Drug Control,Chengdu 611731,China;Dechang People’s Hospital,Liangshan 615500,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第8期1481-1489,共9页
Chinese Journal of Pharmaceutical Analysis
基金
“重大新药创制”科技重大专项(2017ZX09101001)。
