洗涤用品中5种荧光增白剂的高效液相色谱法检测及质谱确证  

Simultaneous determination of five fluorescent bleachers in washing products by high performance liquid chromatography and liquid chromatography-tandem mass spectrometry

作　　者：马会娟[1] 马强[1] 白桦[1] 李晶瑞[1] 孟宪双[1] 陈云霞[1] 李文涛[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123

出　　处：《分析试验室》2014年第5期569-573,共5页Chinese Journal of Analysis Laboratory

基　　金：质检公益性行业科研专项项目(2012104013-9);国家科技支撑计划项目(2013BAK04B03)资助

摘　　要：建立了同时测定洗涤用品中5种荧光增白剂类化合物（荧光增白剂393、荧光增白剂KCB、荧光增白剂CBS-127、荧光增白剂KSN和荧光增白剂OB）的高效液相色谱分析方法及质谱确证方法。洗涤样品以四氢呋喃为提取溶剂进行超声提取，提取液离心处理后，取上清液经微孔滤膜过滤后测定。采用AgilentEclipseXDB—C18色谱柱（250mm×4．6mm，5μm）分离，以甲醇-水二元流动相梯度洗脱，流速1．0mL／min，柱温25℃，荧光增白剂KCB和荧光增白剂CBS-127的检测波长为359nm，荧光增白剂393、荧光增白剂KSN和荧光增白剂OB的检测波长为372nm。荧光增白剂393的定量限为0．25mg／kg，荧光增白剂KCB、荧光增白剂CBS-127、荧光增白剂KSN和荧光增白剂OB的定量限为O．5mg／kg。在低、中、高3种加标水平下的平均回收率为87．8％-103．7％，相对标准偏差为1．5％～4．4％。方法的日内RSD均小于l％，日间RSD均小于2％。适用于洗涤用品中5种荧光增白剂类化合物的测定。The high performance liquid chromatographic （HPLC） and liquid chromatography tandem mass spectrometric （LC-MS/MS） methods were developed for the simultaneous determination of 5 fluorescent bleachers （ Fluorescent Bleacher 393, Fluorescent Bleacher KCB, Fluorescent Bleacher CBS - 127, Fluorescent Bleacher KSN and Fluorescent Bleacher OB） in washing products. The samples were ultrasonically extracted with tetrahydrofuran. The extract was centrifuged. The supernatant was filtered through a membrane and then separated on an Agilent Eclipse XDB-Cls chromatographic column （250 mm x 4. 6 mm, 5 ixm） by gradient elution at a flow rate of 1.0 mL/min with methanol-water as mobile phases. The column temperature was 25 ~C. The wavelength of detection for Fluorescent Bleacher KCB and Fluorescent Bleacher CBS - 127 was 359 nm, but for Fluorescent Bleacher 393, Fluorescent Bleacher KSN and Fluorescent Bleacher OB was 372 nm. The limits of quantitation （LOQs） were 0. 25 mg/kg for Fluorescent Bleacher 393 and 0. 5 mg/kg for Fluorescent Bleacher KCB, Fluorescent Bleacher CBS - 127, Fluorescent Bleacher KSN and Fluorescent Bleacher OB. The mean recoveries at three spiked levels were in the range of 87.8% - 103.7% with the relative standard deviations （RSDs） of 1.5% - 4. 4%. In this method, the intra-day precision was less than 1%, and the inter-day precision was less than 2%. The method was suitable for the determination of 5 fluorescent bleachers in washing products.

关 键 词：高效液相色谱 液相色谱-串联质谱 荧光增白剂 洗涤用品 

分 类 号：O657.7[理学—分析化学]