摘要
建立了邻苯二甲醛(OPA)、对氯间二甲基苯酚(PCMX)和三氯生3种杀菌剂同时分离测定的胶束电动毛细管色谱(MEKC)新方法。详细研究了影响上述3种杀菌剂同时分离与准确定量的因素:如分离缓冲溶液的浓度及pH,十二烷基硫酸钠(SDS)浓度、样品缓冲溶液等。以40.2 cm(有效长度:30 cm)×50μm未涂层熔融石英毛细管为分离柱,20 mmol/L硼砂-80 mmol/L SDS(无需调pH)为分离缓冲溶液,2 mmol/L硼砂-8 mmol/L SDS(含体积分数为10%甲醇)为样品缓冲溶液,检测波长为214 nm。3种杀菌剂的校正峰面积的相对标准偏差(RSD)在1.1%～3.8%范围内,迁移时间的RSD均小于0.9%,OPA、PCMX和三氯生的检出限(LOD,信噪比为3)分别为4.0、0.4、0.4 mg/L,定量限(LOQ,信噪比为10)分别为12、1.2、1.2 mg/L,校正峰面积与相应的质量浓度分别在12～2000 mg/L、1.2～200 mg/L和1.2～200 mg/L范围内具有良好的线性关系,相关系数分别为0.999 4、0.999 3和0.999 5。该法前处理简单,可快速、准确地同时测定3种组分,非常适合常规实验室分析。
A novel method for the separation and determination of o-phthalaldehyde （ OPA）, p- chloro-m-xylenol （PCMX） and triclosan in daily chemicals and compound chemical disinfect- ants in a single run by micellar electrokinetic chromatography （MEKC） was established. The factors such as the buffer concentration and pH, the concentration of sodium dodecyl sulfate （ SDS）, and the sample buffer, were investigated in detail. The analysis was carried out using a 50 μm uncoated capillary of 40.2 cm in total length （effective length： 30 cm）. The running buffer was 20 mmol/L Na2B4O7 and 80 mmol/L SDS. The sample buffer was 2 mmol/L Na2B4O7-8 mmol/L SDS （without pH adjustment） containing 10% （v/v） methanol. The detec- tion wavelength was 214 nm. The relative standard deviations （RSDs） of the corrected peak areas of the three components were in the range of 1. 1% - 3.8%, and the RSDs of migration times were less than 0.9%. The limits of detection （ LODs, S/N = 3 ） were 4.0, 0.4 and 0.4 mg/L, and the limits of quantification （LOQs, S/N= 10） were 12, 1.2, and 1.2 mg/L for OPA, PCMX and triclosan, respectively. The corrected peak areas and the concentrations of the three components showed good linear relationship within the ranges of 12 - 2 000 mg/L, 1. 2 - 200 mg/L and 1.2 - 200 mg/L with the correlation coefficients of 0. 999 4, 0. 999 3 and 0. 999 5 for OPA, PCMX and triclosan, respectively. The method was used for the determination of the three components in compound chemical disinfectants, hand washing liquids, soaps and a toothpaste. The results showed that the three components could be assayed in a single run with simple sample pretreatment, rapidity, accuracy and low cost, and the method is convenient for routine analysis.
出处
《色谱》
CAS
CSCD
北大核心
2013年第1期64-70,共7页
Chinese Journal of Chromatography
关键词
胶束电动毛细管色谱
邻苯二甲醛
对氯间二甲基苯酚
三氯生
杀菌剂
消毒剂
日用化学品
micellar electrokinetic chromatography （ MEKC ）
o-phthalaldehyde （OPA）
p-chloro-m-xylenol （PCMX）
triclosan
bactericides
disinfectant
daily chemical
