摘要
针对烷基酚(Alkylphenol, AP)及烷基酚聚氧乙烯醚(Alkylphenol ethoxylates, APEO)测试方法回收率低、精密度差等问题,利用烷基酚和烷基酚聚氧乙烯醚在反向色谱中不同碳原子聚合物共流的特点,采用液相色谱荧光检测器联用技术建立羽绒中AP和APEO残留量测试方法。研究发现:超声波萃取优于微波萃取、索氏萃取;液相色谱参数为:15 cm C18色谱柱,流动相A泵V(甲醇)∶V(乙腈)∶V(水)为79∶7∶23,流速0.8 mL/min, B泵甲醇,流速0.2 mL/min,等度洗脱,可以实现AP和APEO中辛基酚(Octylphenol, OP)、壬基酚(Nonylphenol, NP)、辛基酚聚氧乙烯醚(Octaphenyl Polyoxyethyiene, OPnEO)、壬基酚聚氧乙烯醚(Nonyl phenoxypolyethoxylethanol, NPnEO)完全分离;该检测方法下OP、NP线性范围为0~9 mg/kg, OPnEO、NPnEO为0~5 mg/kg,相关系数均大于0.998,OP、OPnEO、NP、NPnEO最低检出限分别为0.012、0.018、0.042、0.053 mg/kg,精密度分别为2.58%、4.06%、1.14%、4.64%,回收率分别为96.00%、93.50%、97.00%、101.5%。
In order to solve the problems of low recovery and poor precision of current test methods for alkylphenol and alkylphenol polyoxyethylene ether,based on the Co-flow characteristics of different carbon atom polymers of AP and APEO in reverse chromatography,a method for determination of AP and APEO residues in down were developed by use of a liquid chromatography fluorescence detector.The resulTSshow that ultrasonic extraction is superior to microwave extraction and Soxhlet extraction.Chromatographic conditions are 15 cm C18 chromatographic column,pump A:methanol:acetonitrile:water of 79∶7∶23,flow rate of 0.8 mL/min,pump B of methanol,flow rate of 0.2 mL/min,isocratic elution.OP,NP,OPnEO and NPnEO can completely separate in AP and APEO.The linear range of OP and NP is 0-9 mg/kg OPnEO and NPnEO is 0-5 mg/kg.The correlation coefficienTSare greater than 0.991.The detection rates are 0.012,0.018,0.042 and 0.053 mg/kg for OP,OPnEO,NP,NPnEO.The precisions are 2.58%,4.06%,1.14%and 4.64%for OP,OPnEO,NP,NPnEO.and the recovery are 96.00%,93.50%,97.00%and 101.5%for OP,OPnEO,NP,NPnEO.
作者
丁力进
白洁
孙峰
张妍琰
顾伟
DING Lijin;BAI Jie;SUN Feng;ZHANG Yanyan;GU Wei(Suzhou Institute of Fiber Inspection,Suzhou,Jiangsu 215128,China;China Textile Engineering Society,Beijing 100025,China)
出处
《毛纺科技》
CAS
北大核心
2022年第11期27-32,共6页
Wool Textile Journal
关键词
烷基酚
烷基酚聚氧乙烯醚
氢键
超声波萃取
甲醇
乙腈
alkylphenol
alkylphenol ethoxylates
hydrogen bond
ultrasonic extraction
methanol
acetonitrile
