离子对色谱-抑制电导法测定6-溴己基三甲基溴化铵中相关物质  

Determination of Related Substances in 6-Bromohexyltrimethylaminium Bromide by Ion-Pair Chromatography Suppressed Conductivity Method

作　　者：郑秀瑾 梁晨 严云丽 张彬彬 ZHENG Xiujin;LIANG Chen;YAN Yunli;ZHANG Binbin(Qingdao Shenghan Chromatogram Technology Co.,Ltd,Qingdao 266101)

机构地区：[1]青岛盛瀚色谱技术有限公司,山东青岛266101

出　　处：《分析科学学报》2023年第4期487-491,共5页Journal of Analytical Science

摘　　要：建立了离子对色谱法测定6-溴己基三甲基溴化铵中相关物质的分析方法。样品经超纯水溶解后过0.22μm滤膜进样分析,选用Shinesil C18色谱柱进行色谱分离,高氯酸和乙腈作为淋洗液进行梯度洗脱,采用电导检测器检测,外标法定量。结果表明,6-溴己基三甲基溴化铵和溴化六甲铵的峰面积与其质量浓度在一定范围内呈良好线性关系,检出限分别为1.076 mg/L、0.2327 mg/L,定量限分别为3.587 mg/L、0.7757 mg/L。以6-溴己基三甲基溴化铵样品进行加标回收试验,回收率在95.8%~103.3%之间,测定值的相对标准偏差(RSD,n=6)均小于1.10%。该方法简单快速,可用于6-溴己基三甲基溴化铵样品中主成分6-溴己基三甲基溴化铵和杂质溴化六甲铵的定性和定量分析。A method based on ion-pair chromatography was developed for determination of the related substances in 6-Bromohexyltrimethylaminium bromide.The sample was dissolved with ultrapure water,filtrated with 0.22μm membrane.A Shinesil C18 was selected as the separation column.Perchloric acid solution and acetonitrile were used as the mobile phase in gradient elution.The constituents of sample were analyzed by a conductivity detector,and quantified by an external standard method.As shown by the results,the peak areas of 6-Bromohexyltrimethylaminium bromide and hexamthonium bromide presented a good linear relationship in definite ranges of mass concentration.The limits of detection were 1.076 mg/L and 0.2327 mg/L,respectively.The limits of quantitation were 3.587 mg/L and 0.7757 mg/L,respectively.The recoveries were in the range of 95.8%-103.3%,and RSDs(n=6)were less than 1.10%.A simple and quick method was suitable for qualitative and quantitative analysis of 6-Bromohexyltrimethylaminium bromide(the main ingredient)and hexamthonium bromide(the impurity component)in sample.

关 键 词：离子对色谱法 6-溴己基三甲基溴化铵 溴化六甲铵 

分 类 号：O657.7[理学—分析化学] TM912[理学—化学]