皮革及纺织品中烷基酚与烷基酚聚氧乙烯醚的液相色谱-质谱测定  

Rapid Determination of Alkylphenol and Alkylphenol Ethoxylates in Leather and Textile by Ultrasonic-assisted Extraction and LC-MS

作　　者：温裕云[1,2] 欧延 洪小燕[2] 弓振斌[1,2] 

机构地区：[1]厦门大学近海海洋环境科学国家重点实验室,福建厦门361005 [2]厦门大学海洋与环境学院,福建厦门361005 [3]远东技术服务有限公司,福建泉州362000

出　　处：《分析测试学报》2010年第2期189-193,共5页Journal of Instrumental Analysis

基　　金：福建省自然科学基金重点资助项目(B0220001);远东技术服务有限公司委托项目

摘　　要：建立了液相色谱-质谱法测定皮革及纺织品中辛基酚（OP）、壬基酚（NP）、辛基酚聚氧乙烯醚（OPEO）及壬基酚聚氧乙烯醚（NPEO）的分析方法。样品经超声波振荡萃取，c18反相色谱柱进行分离，甲醇-水为流动相，离子源为ESI。OP和NP采用负离子模式，定量离子分别为m／z205、219；OPEO和NPEO采用正离子模式，定量离子分别为m／z229＋44nEO和m／z243＋44nEO（nEO=3～16）。在优化实验条件下，方法的定量下限为0．25～2．5mg／kg，样品加标回收率为92％～107％，相对标准偏差为5．3％～9．5％（50mg／kg，n=6）。方法简单、快速、灵敏度高，可满足欧盟等地区对皮革及纺织品中OP、NP、OPEO、NPEO的测定要求。A rapid and simple method was developed for measurement of octylphenol （ OP）, nonly phenol（NP）, polyoxyethylene oetylphenol ether （OPEO） and polyoxyethylene nonylphenol ether （NPEO） residues in leather, leather products and textile products, by ultrasonic-assisted extraction and liquid chromatography - mass spectrometry. The analytes were sequentially extracted with 20, 20 and 10 mL methanol, and then separated on a C18 column by gradient elution with methanol -water as mobile phase. OP and NP were quantitatively detected with negative-ion electro-spray ionization at m/z 205 and m/z 219, and OPEO and NPEO were measured with positive-ion electro-spray ionization at m/z 229 ＋ 44nEo and m/z 243 ＋ 44nEo （nEO = 3 -- 16）. The result indicated that under the optimized conditions, the spiked recoveries were in the range of 92% - 107% , and the relative standard deviations（RSDs） for concentration of 50 mg/kg were between 5.3% and 9.5% （n =6）. The quantitation limits were 0. 25 -2.5 mg/kg. The method was simple, rapid and sensitive, and could meet the relevant requirement of European Union.

关 键 词：液相色谱-质谱 皮革及皮革制品 纺织品 烷基酚 烷基酚聚氧乙烯醚 超声波萃取 

分 类 号：O657.63[理学—分析化学]