摘要
建立了固相萃取净化结合超高效液相色谱-二极管阵列检测器(UPLC-DAD)同时检测洗衣液、洗衣粉等洗涤用品中荧光增白剂351、85、28和71的分析方法。样品经2%(体积分数)甲酸水溶液-甲醇提取,经WAX固相萃取小柱净化后,采用Phenomenex Synergi Max-RP色谱柱(150 mm×2.0 mm),以乙腈-10 mmol/L乙酸铵为流动相实现待测物(包括顺式和反式异构体)的良好分离,以二极管阵列检测器检测,结合保留时间和光谱图定性,以标准曲线定量。结果表明,4种荧光增白剂在0.05～180 mg/L范围内线性关系良好,相关系数均大于0.999 3;方法定量限(S/N=10)为1.5～15 mg/kg;添加水平为5～1 500 mg/kg时,回收率为84.9%～105%,相对标准偏差(RSD,n=6)为3.2%～6.1%。应用本方法分析了15个样品,阳性样品检出率为53.3%。该法前处理简单,回收率高,精密度好,适用于洗涤用品中4种荧光增白剂的测定。
A new method was established to determine three stilbene-type disulfonate and one distyrylbiphenyl-type fluorescent whitening agents （ FWA351, FWA85, FWA28 and FWAT1 ） in laundry detergents by solid phase extraction （SPE） and ultra-high performance liquid chromatography with a diode array detector （UPLC-DAD）. The fluorescent whitening agents were extracted from laundry detergents with 2% formic acid aqueous solution and methanol, and purified by WAX SPE colunm, and analyzed by UPLC-DAD on a Phenomenex Synergi Max-RP column （ 150 mmx 2.0 ram）, employing acetonitrile-10 mmol/L ammonium acetate as the mobile phase in a gradient elution mode. The fluorescent whitening agents were qualitatively determined by retention time, and confirmed by the ultraviolet spectrum. The results indicated that the target analytes were in the range of 0.05 - greater than 0. 999 3, and the method limits of 180 mg/L with the correlation coefficients （r） quantification （MLOQ） of target analytes were ranged front 1.5 mg/kg to 15 mg/kg （S/N = 10）. The feasibility of this method was demonstra- ted by the determination of FWAs in samples with spiked recoveries. The recoveries were in the range between 84.9% and 105%, and the precision （relative standard deviation, RSD） ranged from 3.2% to 6. 1% （n =6）. Among the 15 samples analyzed, the rate of positive samples was 53.3%, over 1 000 mg/kg of FWA351 and FWA71 were detected. The method is simple, precise and has high recoveries for the determination of fluorescent whitening agents in laundry detergent samples.
出处
《色谱》
CAS
CSCD
北大核心
2013年第2期162-169,共8页
Chinese Journal of Chromatography
基金
国家质检总局科技项目(2009QK325)
关键词
固相萃取
超高效液相色谱-二极管阵列检测器
荧光增白剂
洗涤用品
solid-phase extraction （SPE）
ultra-high performance liquid chromatographydiode array detector （UPLC-DAD）
fluorescent whitening agents （FWAs）
laundry detergents
