摘要
目的建立尿液中类雌激素（壬基酚（NP）、辛基酚（OP）和双酚A（BPA））的HPLC-荧光测定方法。方法采用β-葡萄糖酸酐酶、硫酸酯酶水解人尿液中的结合型壬基酚、辛基酚和双酚A，酶解后溶液采用OASIS HLB固相萃取柱浓缩、畜集和净化。Watersx Terra^TM MS C18液相色谱柱分离，甲醇＋水作为流动相梯度洗脱。荧光检测，激发波长：225nm；发射波长：310nm。结果NP、OP和BPA具有良好的线性关系，BPA、NP和OP的检出限分别为3．7、4、9和7．5ng／ml，BPA、NP和OP加标回收率分别为：70．2％-95．7％、73．2％～108、2％和76．3％～109．1％；船D分别为5．61％～8．19％、6．01％～7．98％和6、23％～8．61％。结论该方法测定尿液中类雌激素（BPA、OP和NP），具有较高的灵敏度和选择性，结果准确可靠、重现性好。
Objective A comprehensive analytical method based on high performance liquid chromatography fluorescence detection （HPLC-FL） was established to determine BPA, NP and OP in urine. Method The urine samples were de-conjugated by adding β-glucuronidase and sulfatase. After enzymatic treatment, the samples were subjected to the OASIS HLB column solid extraction cartridges to clean-up and concentrate. The HPLC used Waters XTerraTM MS C18 column, a mixture of methanol： water as mobile phase, fluorescence detector with the excitation and emission wavelength at 225 nm and 310 nm, respectively. Results There was good linear relationship. The detection limits of BPA, OP and NP were 3.7 ng/ml, 4.9 ng/ml and 7.5 ng/ml, respectively. The recoveries of BPA, OP and NP were 70.2% - 95.7%, 73.2% - 108.2% and 76.3% - 109.1%, respectively; The precisions were 5.61% - 8.19%, 6.01% - 7.98% and 6.23% - 8.61%, respectively. Conclusion The results showed that the method was simple, sensitive and selective, and suitable for the determination of NP, OP and BPA in urine.
出处
《中国食品卫生杂志》
2008年第2期111-114,共4页
Chinese Journal of Food Hygiene
基金
“十一五”国家科技支撑计划食品安全关键技术重大项目,化学污染物暴露评估技术研究(2006BAK02A01)
关键词
酚类
尿
雌激素类
色谱法
高压液相
Phenols
Urine
Estrogens
Chromatography, High pressure Liquid
