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作 者:刘艳琴[1] 王浩[1] 杨红梅[1] 史海良[1] 郭启雷[1]
机构地区:[1]北京市海淀区产品质量监督检验所,北京100094
出 处:《色谱》2011年第5期458-461,共4页Chinese Journal of Chromatography
基 金:国家质量监督检验总局质量检验公益性行业科研专项项目(200910267-02)
摘 要:建立了采用高效液相色谱-二极管阵列检测器(HPLC-DAD)同时检测化妆品中3种苯扎氯铵同系物(n-C12H25-C9H13NCl、n-C14H29-C9H13NCl、n-C16 H33-C9H13 NCl)的方法。采用含0.5%甲酸的甲醇超声提取样品,以CAPCELL PAK SCX色谱柱(250 mm×4.6 mm,5μm)分离,流动相为40 mmol/L乙酸铵水溶液(含0.1%三乙胺,pH 4.0)和乙腈,梯度洗脱,流速1.0 mL/min,检测波长260 nm,柱温25℃,进样量20μL。该方法的检出限50.0 mg/kg,定量限200.0 mg/kg,线性范围5.0~3 000.0 mg/L,加标回收率92.5%~102.1%,相对标准偏差为3.81%~6.66%。结果表明,该方法快速、准确,能够同时测定化妆品中3种苯扎氯铵同系物。An analytical method based on high performance liquid chromatography with a diode array detector(HPLC-DAD) has been established for the simultaneous determination of 3 benzalkonium chloride homologs(n-C12H25-C9H13NCl,n-C14H29-C9H13NCl,n-C16H33-C9H13NCl) in cosmetics.The sample was extracted with methanol(including 0.5% formic acid) under ultrasonic operation,the HPLC separation was carried out on a CAPCELL PAK SCX column(250 mm×4.6 mm,5 μm),the mobile phases were 40 mmol/L ammonium acetate solution(including 0.1% triethylamine) and acetonitrile with gradient elution,the flow rate was 1.0 mL/min,the detection wavelength was 260 nm,the column temperature was 25 ℃,and the injection volume was 20 μL.The limit of detection was 50.0 mg/kg and the quantitation limit was 200.0 mg/kg for 3 benzalkonium chloride homologs in cosmetics.The linear plots were obtained between 5.0 mg/L and 3 000.0 mg/L.Overall recoveries were between 92.5% and 102.1% with the relative standard deviations(RSDs) between 3.81% and 6.66%.The method is simple,rapid,accurate and suitable for the determination of 3 benzalkonium chloride homologs in cosmetics.
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