色谱

色谱 ›› 2018, Vol. 36 ›› Issue (9): 931-937.DOI: 10.3724/SP.J.1123.2018.04003

• 研究论文 • 上一篇    下一篇

基于均匀和正交试验设计的胶束电动毛细管色谱法同时测定消毒剂和抗抑菌产品中3种核苷类抗病毒药物

王萍1,2, 李梦琦3, 赵丽媛3, 杨屹3, 丁晓静1,2   

  1. 1. 北京市疾病预防控制中心, 北京 100013;
    2. 北京市预防医学研究中心, 北京 100013;
    3. 北京化工大学理学院, 北京 100029
  • 收稿日期:2018-04-01 出版日期:2018-09-08 发布日期:2014-08-05
  • 通讯作者: 丁晓静,E-mail:dxj666@aliyun.com
  • 基金资助:

    国家卫生和计划生育委员会法制司项目（20171704）.

Uniform and orthogonal designs on experimental design and optimization of micellar electrokinetic capillary chromatographic method for the simultaneous analysis of three nucleoside antivirus drugs in disinfectant and anti/bacteriostatic products

WANG Ping1,2, LI Mengqi3, ZHAO Liyuan3, YANG Yi3, DING Xiaojing1,2   

  1. 1. Beijing Center for Disease Control and Prevention, Beijing 100013, China;
    2. Beijing Research Center for Preventive Medicine, Beijing 100013, China;
    3. College of Science, Beijing University of Chemical Technology, Beijing 100029, China
  • Received:2018-04-01 Online:2018-09-08 Published:2014-08-05
  • Supported by:

    Project for Department of Law and Legislation, National Health and Family Planning Commission of the Peoples's Republic of China (No. 20171704).

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摘要：

为防止消毒剂与抗抑菌产品中违规添加核苷类抗病毒药物，建立了胶束电动毛细管色谱（MEKC）同时分离测定消毒剂与抗抑菌产品中3种核苷类抗病毒药物（更昔洛韦、阿昔洛韦和喷昔洛韦）的新方法。通过3因素7水平均匀试验设计和4因素4水平的正交试验设计优化了十二烷基硫酸钠（SDS）、磷酸二氢钠（NaH2PO4）及硼砂（Na2B4O7）在分离缓冲液中的浓度，最大限度地实现了3种核苷类抗病毒药物在短时间内的有效分离。以30.2 cm×50 μ m（有效长度为20 cm）未涂层熔融石英毛细管为分离柱，以25 mmol/L NaH2PO4+10 mmol/L Na2B4O7（pH 7.41）+140 mmol/L（SDS）为分离缓冲溶液，分离电压为10 kV；进样压力为0.003 Pa，进样时间为4 s；检测波长为250 nm。3种抗病毒药物在一定的浓度范围内线性关系良好，相关系数r均不小于0.9995。3种抗病毒药物的检出限均为2.0 mg/kg，定量限均为7.0 mg/kg。低、中、高浓度加标回收率为85.4%~104.1%，相对标准偏差（RSD）均小于8.0%。该方法简便，快速，适于检测消毒剂与抗抑菌产品中更昔洛韦、阿昔洛韦和喷昔洛韦。

关键词: 核苷类抗病毒药物, 胶束电动毛细管色谱, 均匀试验设计, 抗抑菌产品, 消毒剂, 正交试验设计

Abstract:

To prevent the abuse of nucleoside-based antiviral drugs in disinfectant and anti/bacteriostatic products, a new micellar electrokinetic chromatographic (MEKC) method for the simultaneous determination of three nucleoside antiviral drugs (ganciclovir, acyclovir and penciclovir) was established. Three factors and seven levels uniform design and four factors and four levels orthogonal design were used to optimize the concentration of sodium dodecyl sulfate (SDS), sodium dihydrogen phosphate (NaH2PO4) and sodium borate (Na2B4O7) in the running buffer. The three nucleoside antiviral drugs were separated from each other in the shortest time to obtain effective separation through uniform and orthogonal designs on experimental design and optimization. The separation was performed on an uncoated fused-silica capillary with 50 μ m i. d. and a total length of 30.2 cm (effective length:20 cm). An optimized buffer solution consisting of 25 mmol/L NaH2PO4, 10 mmol/L Na2B4O7 (pH 7.41) and 140 mmol/L dodecyl sulfate sodium was used for separation. The applied voltage was 10 kV, the injected pressure and time was at 0.003 Pa for 4 s. The wavelength of the detection was 250 nm. Under the optimum conditions, the corrected area and the concentration had good linearity. The correlation coefficients (r) were not less than 0.9995. The limits of detection were all 2.0 mg/kg. The limits of quantitation were all 7.0 mg/kg. The relative recoveries ranging from 85.4% to 104.1% with RSDs all lower than 8.0%. It showed that the method was suitable for the detection of ganciclovir, acyclovir and penciclovir in disinfectant and anti/bacteriostat products with simplicity and rapidity.

Key words: anti/bacteriostatic products, disinfectant, micellar electrokinetic chromatography (MEKC), nucleoside antiviral drugs, orthogonal experimental design, uniform experimental design

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