纺织学报 ›› 2011, Vol. 32 ›› Issue (11): 90-95.

• 染整与化学品 • 上一篇    下一篇

液相色谱二极管阵列荧光法测定羊绒制品中的3种酚类激素

李志刚   

  1. 浙江工业职业技术学院
  • 收稿日期:2010-11-25 修回日期:2011-03-07 出版日期:2011-11-15 发布日期:2011-11-15
  • 通讯作者: 李志刚 E-mail:lzg2010@zjipc.com

Determination of 3 phenolic environmental hormones in cashmere fabrics by HPLC-DAD-FLD

[中]李志刚 [英]LI Zhi-Gang   

  • Received:2010-11-25 Revised:2011-03-07 Online:2011-11-15 Published:2011-11-15
  • Contact: [中]李志刚 [英]LI Zhi-Gang E-mail:lzg2010@zjipc.com

摘要: 建立了羊绒织品中双酚A、4-壬基酚和辛基酚等3种酚类环境激素的高效液相色谱二极管阵列荧光串联检测方法。样品经索氏提取后,在Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d., 2.2 μm)快速柱上分离,采用甲醇+乙腈+ 水(30+50+20, V/V/V)为流动相,紫外检测波长为225 nm,荧光检测激发波长λex 228 nm,发射波长λem 305 nm,外标法定量。实验结果表明:3种环境激素荧光检测在0.01~1.0 mg/kg的浓度范围内呈良好的线性关系,定量检测下限为0.01 mg/kg。紫外检测在0.05~10.0 mg/kg的浓度范围内呈良好的线性关系,定量检测下限为0.05 mg/kg。方法回收率在82.0~102.0%之间,平均回收率为89.2%,RSD 为1.8~7.5% 。本方法简便、灵敏、重现性好、干扰少,能满足羊绒织品中双酚A、4-壬基酚和辛基酚残留的测定要求。

Abstract: A method for determination of phenolic environmental hormones such as bisphenol A , 4-nonylphenol and octylphenol in cashmere fabrics by high performance liquid chromatography with diode array detector and fluorescence detector (HPLC-DAD-FLD) was established. After cashmere fabrics were extracted by Soxhlet Extraction, the extracts were separated and eluted on a fast chromatographic column ,Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d., 2.2 μm)by using the mobile phase consisting of CH3OH+CH3CN+H2O (30+50+20, V/V/V) . Detection was performed by DAD at 225 nm and FLD at λex 228 nm, λem 305 nm using extenal standard method. The result of experiment indicates that calibration curves of 3 phenolic environmental hormones were linear within the range of 0.01~1.0 mg/kg for FLD, the limits of quantification were found to be 0.01 mg/kg. Calibration curves were linear within the range of 0.05~10.0 mg/kg for UV, the limits of quantification were 0.05 mg/kg for them. The extraction recoveries were between 82.0~102.0% and the average recovery was 89.2%, the RSD was 1.8~7.5%. This method is found to be simple, sensitive, accurate, little interferential for the determination of bisphenol A , 4- nonylphenol and octylphenol residue in cashmere fabrics.

中图分类号: 

  • TS 190.2
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