摘要
目的:建立同时测定药用卤化丁基胶塞中2,6-二叔丁基对甲酚(BHT)、游离硫、抗氧剂1010、抗氧剂330、抗氧剂1076、抗氧剂168含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent Zorbax SB-C18,流动相为甲醇-水(梯度洗脱),流速为1.0m L/min,柱温为25℃,检测波长为220 nm,进样量为10μL。结果:BHT、游离硫、抗氧剂1010、抗氧剂330、抗氧剂1076、抗氧剂168的检测质量浓度线性范围分别为2.592~64.80μg/m L(r=0.999 9)、2.648~66.20μg/m L(r=0.999 9)、2.062~51.55μg/m L(r=0.999 9)、2.654~66.35μg/m L(r=0.999 9)、2.128~53.20μg/m L(r=0.999 9)、2.468~61.70μg/m L(r=0.999 9);定量限分别为2.073 6、2.118 4、2.749 2、1.061 6、4.436 0、3.090 4 mg/kg,检测限分别为0.628 4、0.641 9、0.833 1、0.321 7、1.344 2、0.992 4 mg/kg;精密度、稳定性、重复性试验的RSD均小于3%;加样回收率分别为96.57%~99.17%(RSD=0.92%,n=9)、77.47%~86.14%(RSD=2.94%,n=9)、96.11%~98.39%(RSD=0.63%,n=9)、96.22%~98.33%(RSD=0.67%,n=9)、95.59%~99.22%(RSD=1.11%,n=9)、81.54%~88.31%(RSD=2.46%,n=9)。结论:该方法灵敏快速、操作简便、重复性好,可用于同时测定药用卤化丁基胶塞中5种抗氧剂和游离硫的含量。
OBJECTIVE:To establish a method for simultaneous determination of BHT,free sulfur,antioxidant 1010,antioxidant 330,antioxidant 1076 and antioxidant 168 in pharmaceutical halogenated butyl rubber stopper.METHODS:HPLC method was adopted.The determination was performed on Agilent Zorbax SB-C18 column with mobile phase consisted of methanol-water(gradient elution)at the flow rate of 1.0 mL/min.The column temperature was 25℃,and detection wavelength was set at 220 nm.The sample size was 10μL.RESULTS:The linear ranges of BHT,free sulfur,antioxidant 1010,antioxidant 330,antioxidant 1076 and antioxidant 168 were 2.592-64.80μg/mL(r=0.999 9),2.648-66.20μg/mL(r=0.999 9),2.062-51.55μg/mL(r=0.999 9),2.654-66.35μg/mL(r=0.999 9),2.128-53.20μg/mL(r=0.999 9),2.468-61.70μg/mL(r=0.999 9),respectively.The limits of quantitation were 2.073 6,2.118 4,2.749 2,1.061 6,4.436 0,3.090 4 mg/kg;the limits of detection were 0.628 4,0.641 9,0.833 1,0.321 7,1.344 2,0.992 4 mg/kg,respectively.RSDs of precision,stability and reproducibility tests were all lower than 3%.The average recoveries were 96.57%-99.17%(RSD=0.92%,n=9),77.47%-86.14%(RSD=2.94%,n=9),96.11%-98.39%(RSD=0.63%,n=9),96.22%-98.33%(RSD=0.67%,n=9),95.59%-99.22%(RSD=1.11%,n=9)and 81.54%-88.31%(RSD=2.46%,n=9),respectively.CONCLUSIONS:The method is sensitive,rapid,convenient and reproducible,and can be used for simultaneous determination of 5 antioxidant and free sulfur in pharmaceutical halogenated butyl rubber stopper.
作者
朱碧君
李婷婷
孙会敏
胡星宇
何君怡
罗跃华
ZHU Bijun;LI Tingting;SUN Huimin;HU Xingyu;HE Junyi;LUO Yuehua(Jiangxi Institute for Drug Control/Jiangxi Drug and Medical Devices Quality Engineering Research Center,Nanchang 330029,China;Chengdu Institute for Food and Drug Control,Chengdu 610045,China;National Institute for Food and Drug Control,Beijing 100050,China;School of Graduate,Jiangxi University of TCM,Nanchang 330006,China;The Affiliated Yangpu Hospital of Tongji University,Shanghai 200090,China)
出处
《中国药房》
CAS
北大核心
2018年第18期2475-2479,共5页
China Pharmacy
基金
国家自然科学基金资助项目(No.81373955)
江西省食品药品监督管理局科技计划项目(No.2015yp07)
