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作 者:宋宝花[1,2] 丁晓静[1,3] 李佳[1,3] 王志[2]
机构地区:[1]北京市疾病预防控制中心,北京100013 [2]河北农业大学理学院,河北保定071001 [3]首都医科大学公共卫生与家庭医学学院,北京100069
出 处:《色谱》2012年第9期943-950,共8页Chinese Journal of Chromatography
摘 要:建立了复方化学消毒剂中常用有效成分醋酸洗必泰和苯扎氯铵(C12-BAC、C14-BAC及C16-BAC)同时分离测定的毛细管电泳(CE)方法。以37 cm×50μm未涂层熔融石英毛细管为分离柱,以150 mmol/L磷酸二氢钠-62.5mmol/L磷酸(pH 2.5)缓冲液(含体积分数为40%的乙腈)为分离缓冲溶液,50 mmol/L醋酸-乙腈(体积比为1∶1)为样品介质,检测波长为214 nm。方法的日内及日间精密度分别小于3.0%及3.7%。醋酸洗必泰、C12-BAC、C14-BAC及C16-BAC的检出限(信噪比为3)分别为0.3、0.5、0.5、0.5 mg/L,定量限(信噪比为10)分别为1.0、1.5、1.5和1.5 mg/L,在1.0~400、1.5~200、1.5~200和1.5~200 mg/L范围内,4种有效成分的校正峰面积与相应质量浓度均具有良好的线性关系,相关系数分别为0.999 5、0.999 8、0.999 7和0.999 8。加标回收率为93.83%~104.97%。将该法用于实际样品分析,并与液相色谱的分析结果进行比对,获得满意结果。Benzalkonium chloride(BAC) is a mixture of alkyl substituted benzyl dimethylammonium chloride homologs(C12-BAC,C14-BAC and C16-BAC).Chlorhexidine acetate is a widely used effective component in compound chemical disinfectants.A method for the simultaneous determination of chlorhexidine acetate and benzalkonium chloride in compound chemical disinfectants by capillary electrophoresis(CE) was established.The CE analysis was carried out using an uncoated capillary with 50 μm i.d.and 37 cm total length.The running buffer was 150 mmol/L NaH2PO4-62.5 mmol/L H3PO4(pH 2.5) containing 40%(v/v) acetonitrile.The sample medium was 50 mmol/L acetic acid-acetonitrile(1∶1,v/v).The detection wavelength was 214 nm.The factors such as the buffer concentration and pH,the content of acetonitrile,which influenced the separation and accurate assay of compound chemical disinfectants were investigated in detail.The intra-day and inter-day precisions of the method were below 3.0% and 3.7%,respectively.The limits of detection(LOD,signal to noise ratio(S/N)=3) for chlorhexidine acetate,C12-BAC,C14-BAC and C16-BAC were 0.3,0.5,0.5 and 0.5 mg/L,respectively.The limits of quantification(LOQ,S/N=10) were 1.0,1.5,1.5,and 1.5 mg/L,respectively.The corrected peak area and the mass concentration of the four components mentioned above showed good linear relationships within the ranges of 1.0-400 mg/L,1.5-200 mg/L,1.5-200 mg/L and 1.5-200 mg/L,with linear correlation coefficients(r) of 0.9995,0.9998,0.9997 and 0.9998,respectively.The established method was used for the determination of the four disinfectants in the compound chemical disinfectants.The results were in good agreement with those obtained by the high performance liquid chromatographic method.
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