复方化学消毒剂中苯扎氯铵的高效液相色谱测定

建立了一种测定复方化学消毒剂中苯扎氯铵成分十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵和十六烷基二甲基苄基氯化铵的反相离子对高效液相色谱法。色谱柱为Platisil ODS(5μm,250 mm×4.6mm),流动相为甲醇-0.2 mol/L己烷磺酸钠(含1%三乙胺,V/V,用高氯酸调节至pH=6.0,体积比85∶15),紫外220 nm检测。用己烷磺酸钠作为离子对试剂,增强了苯扎氯铵成分的保留,三乙胺作为扫尾剂,通过抑制固定相表面残存的硅羟基对苯扎氯铵成分的吸附,减少了色谱峰拖尾。3种苯扎氯铵成分分离良好,标准曲线的线性范围分别为0.002～5 mg/mL、0.005～10 mg/mL和0.005～10 mg/mL,检测限分别为0.0005 mg/mL、0.001mg/mL和0.001 mg/mL。方法具有良好的准确度和精密度,在测定低浓度样品时优势明显。实际用于测定苯扎氯铵消毒液和医用消毒纸巾中3种苯扎氯铵成分的含量,回收率为99.3%～104.1%,日内和日间测定相对标准偏差(RSD)均小于2.0%。

Determination of Benzalkonium Chloride Homologs in Complex Chemical Disinfectant by High-Performance Liquid Chromatography

An ion pair reversed phase High-Performance Liquid Chromatography(HPLC) method has been developed for the simultaneous determination of benzalkonium chloride(BAC) homologues,dodecyl dimethyl benzyl ammonium chloride(C12),tetradecyl dimethyl benzyl ammonium chloride(C14) and cetyl dimethyl benzyl ammonium chloride(C16),in complex chemical disinfectant.Separation was carried out on Platisil ODS column(5 μm,250 mm×4.6 mm),using methanol and 200 mmol/L hexane sulfonate sodium aqueous solution consisting of 1% triethylamine(V/V),adjusted with perchloric acid to pH 6.0(85∶15,V/V) as the mobile phase in an isocratic elution.The detection wavelength was 220 nm.In the experiment,sodium hexanesulfonate was used as the ion-pair reagent to enhance the retention of benzalkonium chloride,and triethylamine was used as the tailing-suppressor to restrain the adsorption of benzalkonium chloride to the residual silanols on the stationary phase surface.Calibration curves for C12,C14 and C16 were linear in the range of 0.002-5 mg/mL,0.005-10 mg/mL and 0.005-10 mg/mL,with the limits of quantifications(LOQs) being 0.0005,0.001 and 0.001 mg/mL,respectively.The method presents excellent accuracy and satisfactory precision,and it has a significant advantage in the detection of low content samples.The average recoveries were in the range of 99.3%-104.1%,and the intra-and inter-day relative standard deviations(RSDs) were not more than 2.0% for the determined compounds in benzalkonium chloride disinfectant and benzalkonium chloride towelette.