硫柳汞中汞离子检查方法.docVIP

硫柳汞中汞离子检查方法[摘要] 目的:建立硫柳汞中汞离子的检查方法。方法:采用紫外分光光度法进行测定。检测波长:323 nm。结果:通过对两种方法的检测灵敏度和限度进行比较,发现国外药典记载紫外分光光度法测定结果可准确的定量为0.60%。结论:采用紫外分光光度法测定硫柳汞中汞离子的方法简单、方便,专属性好。 [关键词] 紫外分光光度法;汞离子;硫柳汞;测定 [中图分类号] R927.2[文献标识码] B[文章编号] 1673-7210(2010)04(a)-094-02 The method for determination of mercury ion in thiomersal GAO Yan1, ZHENG Shuai2, QIU Yilan3 (1.The Hospital in Shahekou District, Dalian City, Dalian 116021,China; 2.The Hospital of International Airport in Zhoushuizi, Dalian 116033,China; 3.Institute for Drug Control of Dalian City, Dalian 116021, China) [Abstract] Objective: To establish a method for the determination of mercury in thiomersalate by UV-spectrophotometric. Methods: UV-spectrophotometric was be used. The detection wavelength was at 323 nm. Results: Compared with of sensitivities and limits of the two methods, we found that the limit concentration of mercury ion in sample was about 0.65% by the method listed in the Ministry of Health Drug Standard, which was nearly as the same as the concentration of 0.6% determined by UV-spectrophotometric. Conclusion: The method is fast, reliable, accurate and can be used in the quality control of mercury ion in thiomersalate. [Key words] UV-spectrophotometric; Mercury ion; Thiomersal; Contend detormination 硫柳汞作为一种药用辅料,长期以来一直被用做生物制品包括许多疫苗的防腐剂,尤其用在多剂量反复取用的药剂瓶中[1]。目前,硫柳汞的安全性还存在争议。由于其生产制备工艺,贮存过程可能带来的游离汞离子具有不容忽视的毒副作用,比如急性中毒、神经系统毒性、肾损伤、免疫损伤、皮肤过敏反应、致癌、生殖胚胎毒性致畸等[2],所以对其中游离汞离子的检查尤为重要。然而目前《中国药典》却没有收载硫柳汞的质量标准,《卫生部药品标准》二部第五册[3]中收录了硫柳汞的质量标准,是由上海市药检所于1996年起草的。本试验就硫柳汞中汞离子的检查项目,参照国内外的质量标准:《美国药典》第32版[4]、《英国药典》2008年版[5]及《欧洲药典》第6版[6]、《卫生部药品标准》二部第五册进行探讨,以确定硫柳汞中汞离子的检查方法。 1 仪器与试药 1.1 仪器 P221S型电子天平(德国Sartorius公司);UV-2401PC型紫外可见分光光度仪(日本岛津公司)。 1.2 试药 硫柳汞(北京益利精细化学有限公司,批号;醋酸汞,碘化钾,硫化亚铁,氯化汞,均为分析纯。氨试液,稀盐酸为自制。 2 方法与结果 2.1 《美国药典》方法 2.1.1 碘试液精密称取碘化钾33.20 g,置100 ml量瓶中,加水75 ml,振摇使之溶解,加水至刻度,摇匀。 2.1.2 对照品溶液制备精密称取氯化汞191.1 mg,置200 ml量瓶中,加水100 ml使溶解并稀释至刻度,摇匀。精密量取上述溶液5 ml置50 ml量瓶中,加水稀释至刻度,摇匀(标准溶液中氯化汞的浓度约为95.55