摘要
建立了羊绒制品中双酚A、4-n-壬基酚和辛基酚3种酚类环境激素的高效液相色谱二极管阵列荧光检测方法。样品经索氏提取后,在Shim-pack XR-ODSⅡ快速色谱柱上分离,采用甲醇/乙腈/水(体积比为30∶50∶20)为流动相,紫外检测波长为225 nm,荧光检测激发波长为228 nm,发射波长为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%。该方法简便、灵敏、重现性好、干扰少,能满足羊绒制品中双酚A、4-n-壬基酚和辛基酚残留的检测要求。
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 by using a mobile phase consisting of CH3OH/CH3CN/H2O（at a volume ratio 30∶50∶20）.Detection was performed by DAD at 225 nm and FLD at 228 nm and 305 nm using extenal standard method.The experimental results indicate that calibration curves of 3 kinds of phenolic environmental hormones were linear within the range of 0.01-1.0 mg/kg for FLD,the lower limit of quantification was found to be 0.01 mg/kg.Calibration curves were linear within the range of 0.05-10.0 mg/kg for UV,the lower limit of quantification was 0.05 mg/kg.The extraction recovey was 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 and little interference for the determination of bisphenol A,4-n-nonylphenol and octylphenol residue in cashmere fabrics.
出处
《纺织学报》
EI
CAS
CSCD
北大核心
2011年第11期90-95,共6页
Journal of Textile Research
