Chao Hsi-Chun, Liao Hsiao-Wei, Kuo Ching-Hua
School of Pharmacy, College of Medicine, National Taiwan University, Taipei, Taiwan.
School of Pharmacy, College of Medicine, National Taiwan University, Taipei, Taiwan; Department of Pharmacy, National Taiwan University Hospital, Taiwan.
J Chromatogr A. 2016 May 6;1445:149-57. doi: 10.1016/j.chroma.2016.03.086. Epub 2016 Apr 1.
Phthalate plasticizers are widely used in the plastics industry, but they have been detected in soft drinks, pharmaceuticals and food products. This study developed a method that uses water plug-assisted analyte focusing by micelle collapse and microemulsion electrokinetic chromatography (WPA-AFMC-MEEKC) for quantifying benzyl butyl phthalate (BBP), dibutyl phthalate (DBP), diethylhexyl phthalate (DEHP), and diisodecyl phthalate (DIDP) in pediatric pharmaceuticals. The AFMC strategy was applied to improve the detection sensitivity, and a short water plug was introduced to assist micelle collapse in the micelle dilution zone for sample stacking. To carry neutral phthalates into the capillary through electrokinetic injection, sodium dodecyl sulfate (SDS) was added to the sample solution, and 8mM SDS was selected as the optimal concentration. The optimized background solution (BGS) contained 16.13mM phosphate buffer (pH=2.5), 150mM SDS, 0.75% n-octane (v/v), 5% 1-butanol (BuOH), 22.5% acetonitrile (ACN), and 15% isopropanol (IPA). Under the optimal separation conditions, four phthalates could be quantified within 20min with enhancement factors of 58, 200, 86 and 90 for DIDP, DEHP, BBP, and DBP, respectively, compared to the conventional MEEKC mode. The limits of detection were within the range of 0.047-0.010μgmL(-1). The accuracy of the method was within the range of 96-117%. The WPA-AFMC-MEEKC method was applied for the analysis of six pediatric pharmaceuticals, and the results demonstrated that the developed method is sensitive and accurate, allowing it to be used for quality control of pediatric pharmaceuticals.
邻苯二甲酸酯类增塑剂在塑料工业中广泛使用，但已在软饮料、药品和食品中被检测到。本研究开发了一种利用水塞辅助胶束塌缩的分析物聚焦和微乳液电动色谱法（WPA-AFMC-MEEKC）来定量儿科药物中邻苯二甲酸苄基丁酯（BBP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-乙基己基）酯（DEHP）和邻苯二甲酸二异癸酯（DIDP）的方法。应用AFMC策略提高检测灵敏度，并引入短水塞以辅助胶束稀释区中的胶束塌缩进行样品堆积。为了通过电动进样将中性邻苯二甲酸酯带入毛细管，在样品溶液中加入十二烷基硫酸钠（SDS），并选择8mM SDS作为最佳浓度。优化后的背景溶液（BGS）包含16.13mM磷酸盐缓冲液（pH=2.5）、150mM SDS、0.75%正辛烷（v/v）、5%正丁醇（BuOH）、22.5%乙腈（ACN）和15%异丙醇（IPA）。在最佳分离条件下，与传统的MEEKC模式相比，四种邻苯二甲酸酯可在20分钟内定量，DIDP、DEHP、BBP和DBP的增强因子分别为58、200、86和90。检测限在0.047-0.010μgmL(-1)范围内。该方法的准确度在96-117%范围内。WPA-AFMC-MEEKC方法应用于六种儿科药物的分析，结果表明所开发的方法灵敏且准确，可用于儿科药物的质量控制。
