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超高效合相色谱法快速筛查卤化丁基橡胶塞中14种抗氧剂OA北大核心CSTPCD

Rapid Determination of 14 Antioxidants in Halogenated Butyl Rubber Stoppers by Ultra-performance Convergence Chromatography

中文摘要英文摘要

目的 建立一种快速检测卤化丁基胶塞中 14 种抗氧剂的方法.方法 采用超高效合相色谱法,色谱柱为ACQUITY UPC2 BEH-2EP(100 mm×3.0 mm,1.7 μm),主要以超临界二氧化碳流体作为流动相,同时以甲醇-乙腈(1∶1)为流动相改性剂进行梯度洗脱,流速 1.5 mL·min-1,系统背压 13.79×103 kPa,柱温 40℃,进样体积 1 μL,检测器为二极管阵列检测器(PDA),检测波长 220 nm.结果 14 种抗氧剂可以在 5 min内实现分离检测.在 5~100 μg·mL-1 范围内,14 种抗氧剂的质量浓度分别与各自峰面积呈现出良好的线性关系,相关系数(r)均>0.998,平均加标回收率为89.80%~102.96%,相对标准偏差(RSD)为 0.4%~2.4%(n=9).对 10 批次卤化丁基胶塞样品进行检测,主要检测到了 4种抗氧剂,分别为抗氧剂BHT、抗氧剂 168、抗氧剂 1076 及抗氧剂 1010.结论 该方法简便高效,选择性非常强,能够准确快速地分析卤化丁基胶塞中的抗氧剂.

Objective To establish a rapid detection method based on ultra-performance convergence chromatography for the analysis of 14 antioxidants in halogenated butyl rubber stoppers.Methods Ultra-performance convergence chromatogra-phy was adopted.The determination was performed on ACQUITY UPC2 BEH-2EP(100 mm×3.0 mm,1.7 μm);Supercritical carbon dioxide fluid and methanol/acetonitrile(1∶1)were used as the gradient elution and the flow rate was 1.5 mL·min-1;the automatic back pressure regulator(ABPR)was 13.79×103 kPa;The column temperature was 40℃;The injection volume was 1 μL;The detection wavelength of the photodiode array detector(PDA)was 220 nm.Results The full baseline separation of the 14 antioxidants was achieved in 5.0 min.14 antioxidants showed good linear relationships within the ranges of 5-100 μg·mL-1,respectively.And the correlation coefficients was above 0.998.The average recoveries were 89.80%-102.96%,and the RSD were 0.4%-2.4%(n=9).The results showed that four antioxidants including antioxidant BHT,168,1076,and 1010 were mainly detected in halogenated butyl rubber stoppers.Conclusion This method is simple,fast,with good selectivity,and suitable for the analysis of the antioxidants in halogenated butyl rubber stoppers.

付蒙;陈晓莉;陈雷霖;曹运姣;胡敏;赵霞

湖北省药品监督检验研究院,湖北省药品质量检测与控制工程技术研究中心,国家药品监督管理局中药质量控制重点实验室,武汉 430075湖北中医药大学,武汉 430065中国食品药品检定研究院,北京 100050

药学

卤化丁基橡胶塞抗氧剂超高效合相色谱法二极管阵列检测器

Halogenated butyl rubber stoppersAntioxidantsUltra-performance convergence chromatographyPhotodi-ode array detector

《医药导报》 2024 (005)

706-711 / 6

湖北省药品监督检验研究院中青年科研基金资助项目(2022YN004).

10.3870/j.issn.1004-0781.2024.05.006

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