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双胶束电动毛细管色谱测定复方化学消毒剂中聚六亚甲基单胍、聚六亚甲基双胍、醋酸洗必泰和苄索氯铵
  • ISSN号:1000-8713
  • 期刊名称:《色谱》
  • 时间:0
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]首都医科大学公共卫生学院,北京100069, [2]北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京100013
  • 相关基金:北京市卫生系统高层次卫生技术人才培养项目(2013-2-036)
中文摘要:

建立了双胶束电动毛细管色谱(MEKC)分离测定复方化学消毒剂中有效成分聚六亚甲基单胍(PHMG)、聚六亚甲基双胍(PHMB)、醋酸洗必泰(CHA)及苄索氯铵(BTC)的新方法。以50.2 cm(有效长度:40 cm)×50μm i.d.未涂层熔融石英毛细管为分离柱,20 mmol/L硼砂+30 mmol/L十二烷基硫酸钠(SDS)+5 mmol/L脱氧胆酸钠(SD)+0.8 g/L聚乙二醇20000为分离缓冲溶液。详细研究了分离缓冲溶液中各组分浓度、样品提取液对分离的影响。4种物质的检出限和定量限均分别为1 mg/L和3 mg/L。4种物质的校正峰面积与相应质量浓度在3~140mg/L范围内,均具有良好的线性关系,相关系数均大于0.999。回收率在84.1%~109.6%间,相对标准偏差(RSD)均低于6%。用该法测定了11件复方化学消毒剂样品中PHMG、PHMB、CHA和BTC,与产品标识值基本吻合。该法可成功区分单胍与双胍,且操作简单,适用于消毒产品的质量监督。

英文摘要:

A new method for the accurate assay of four components(polyhexamethylene guanide(PHMG),polyhexamethylene biguanide(PHMB),chlorhexidine acetate(CHA) and benzethonium chloride(BTC))in compound chemical disinfectants by micellar electrokinetic chromatography(MEKC) with bi-micelle was developed. An uncoated fused-silica capillary with 50 μm i.d. and 50. 2 cm total length(effective length:40 cm)under a separation voltage of 24 kV was used. The separation buffer consisted of 20 mmol / L Na_2B_4O_7,30 mmol/ L sodium dodecyl sulfate(SDS),5 mmol / L sodium deoxycholate(SD)and 0. 8 g / L polyethyleneglycol(PEG)20000. A 1 ∶10 dilution of the running buffer with ultrapure water was used as the sample buffer. The injection pressure and time were 3. 448 kPa and 12 s,respectively. Liquid samples could be directly injected after dilution with sample buffer. Solid samples were extracted with10 mL of sample buffer twice and the two extracted solutions were merged together and then directly injected. The factors such as the buffer concentration and pH,the concentrations of SDS and SD,the concentration of PEG 20000 and the sample extraction solution which influence theseparation were investigated in detail. The corrected peak areas versus the concentrations of the four components showed good linear relationships within the range from 3 mg / L to 140 mg / L with correlation coefficients(r)greater than 0. 999. The limits of detection(LODs)and the limits of quantification(LOQs)of the four components were all 1 mg / L and 3 mg / L,respectively. The average recoveries at three spiked levels were in the range of 84. 1%- 109. 6% with RSDs all less than 6%. Eleven samples were analyzed and the results met well with the specified content. The PHMG could be easily discriminated from PHMB. The MEKC method is suitable for the supervision of compound chemical disinfectants.

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期刊信息
  • 《色谱》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国化学会 中国科学院大连化学物理研究所
  • 主编:张玉奎
  • 地址:大连市中山路457号
  • 邮编:116023
  • 邮箱:sepu@dicp.ac.cn
  • 电话:0411-84379021
  • 国际标准刊号:ISSN:1000-8713
  • 国内统一刊号:ISSN:21-1185/O6
  • 邮发代号:8-43
  • 获奖情况:
  • 1998年获中国科学院科学出版基金择优支持(1998-2...,2001年获第四届中国科学院优秀期刊二等奖,2002年获第三届中国科协优秀期刊三等奖,连续多年被评为辽宁省一级期刊
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),波兰哥白尼索引,荷兰文摘与引文数据库,美国生物医学检索系统,美国剑桥科学文摘,日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:26730