孕马尿中3种主要结合雌激素的固相萃取-UPLC法测定.pdfVIP

中国医药工业杂志 Chinese Joumal of Pharmaceuticals 2011 , 42 (7) • 529 • 能去三EE:〉 孕马尿中 3 种主要结合雌激素的固相萃取-UPLC 法测定 姚军1 ，赵文慧1 ，兰欢1 ，肖建民z，高晓黎l (1.新疆医科大学药学院，新疆乌鲁木齐 830054; 2. 新疆特丰药业股份有限公司，新疆乌鲁木齐83001 1) 摘要:建立了固相萃取-超高效液相色谱法快速检测新疆孕马尿中的3 种主要结合雌激素一一雌嗣硫酸纳、马烯雌嗣硫 酸销和 17α· 双氢马烯雌酣硫酸锅.采用大孔树脂固相萃取柱 (SPE) 富集孕马尿中的结合雌激素，以 UPLC-PDA 检测. 采用 C 0.025 moνL 磷酸二氢饵溶液-乙腊 (77 : 23) 为流动相，检测波长215 nm. 3 种结合雌激素分别在 色谱柱，以 18 0.6-6.0、 0.3 - 3.0 和 0.2 - 2.0μg1m1浓度范围内线性关系良好.平均回收率分别为 97.0% 、 96.4%和 98.3% ， RSD 分 别为 0.9% 、1.7%和1.6% 。 关键词g 孕马尿:结合雌激素:固相萃取:超高效液相色谱g 测定 中图分类号: 0657.72; TQ460.γ2 文献标志码:A 文章编号: 1ω1-8255 (2011)07-0529-03 De阳nination ofThree Main Conjugated Estrogens in Pregnant Mare Urine by SPE-UPLC 1 1 1 1 YAO Jun , ZHAO Wenhui , LAN Huan , XIAO Jianm矿， GAO Xiaoli (1. College ofPharmacy. Xinjiang Medica/ Universi凯， Urumqi 830054; 2. Xinjiang 1拚ng Pharmaceutica/ Compal秽\ Urumqi 830011) ABSTRACT: A solid phase extraction-ultra preference liquid chromatography (SPE-UPLC) method was established for the determination of 也ree main conjugated estrogens: sodium estrone sulfate, sodium equilin sulfate and sodium 17α-dihydroequilin sulfate, in the urine from pregnant Xinjiang m缸e. Macroporous adso叩，tive resin w副 used to enrich the ∞njugated estrogens.Three main conjugated estrogens were eluted by ethanol. The eluent was analyzed by UPLC-PDA. A C 18 column was used with the mobile phase of 0.025 moUL monopotassium phosphate solution- aceωm创le(77 : 23) at the detection waveleng也 of 215 nm. The calibration αlfVes were linear in 也e ranges of 0.6-6.0, 0.3-3.0 and 0.2-2.0μglm1， respectivel予The average recoveries were 97.0% , 96 .4% and 98.3% , with RSDs