HPLC法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
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篇名: HPLC法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
TITLE:
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1.0 mL/min,柱温为25 ℃,检测波长为220 nm,进样量为10 μL。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2.592~64.80 μg/mL(r=0.999 9)、2.648~66.20 μg/mL(r=0.999 9)、2.062~51.55 μg/mL(r=0.999 9)、2.654~66.35 μg/mL(r=0.999 9)、2.128~53.20 μg/mL(r=0.999 9)、2.468~61.70 μg/mL(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。
ABSTRACT: 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 10 μL. RESULTS: The linear ranges of BHT, free sulfur, antioxidant 1010, antioxidant 330, antioxidant 1076 and antioxidant 168 were 2.592-64.80 μg/mL (r=0.999 9), 2.648-66.20 μg/mL (r=0.999 9), 2.062-51.55 μg/mL (r=0.999 9), 2.654-66.35 μg/mL (r=0.999 9), 2.128-53.20 μg/mL (r=0.999 9), 2.468-61.70 μg/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.
期刊: 2018年第29卷第18期
作者: 朱碧君,李婷婷,孙会敏,胡星宇,何君怡,罗跃华
AUTHORS: ZHU Bijun,LI Tingting,SUN Huimin,HU Xingyu,HE Junyi,LUO Yuehua
关键字: 药用卤化丁基胶塞;2,6-二叔丁基对甲酚;游离硫;抗氧剂1010;抗氧剂330;抗氧剂1076;抗氧剂168;高效液相色谱法;含量测定
KEYWORDS: Pharmaceutical halogenated butyl rubber stopper; BHT; Free sulfur; Antioxidant 1010; Antioxidant 330; Antioxidant 1076; Antioxidant 168; HPLC; Content determination
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