固相萃取-高效液相色谱法测定大鼠尿样中调环酸钙  

Determination of Prohexadion-calcium in Urine by Solid Phase Extraction Combined with High Performance Liquid Chromatography

作　　者：马安萍 陈红红 阮小林[2] 丘静静 吴邦华[2] MA An-ping;CHEN Hong-hong;RUAN Xiao-lin;QIU Jing-jing;WU Bang-hua(School of Public Health ,Guangdong Pharmaceutical University ,Guangzhou ,Guangdong 510310;Guangdong Province Hospital for Occupational Disease Prevention and Treatment, Guangzhou, Guangdong 510310)

机构地区：[1]广东药科大学公共卫生学院,广东广州510310 [2]广东省职业病防治院,广东省职业病防治重点实验室,广东广州510310

出　　处：《分析科学学报》2018年第2期291-293,共3页Journal of Analytical Science

摘　　要：建立了大鼠尿样中调环酸钙的高效液相色谱(HPLC)测定方法。样品经Waters OasisMAX 3cc固相萃取小柱净化,Poroshell 120EC-C18色谱柱(100×4.6 mm,2.7μm)分离,甲醇-0.01%甲酸水溶液梯度洗脱,流速为0.4mL/min,检测波长275nm。研究结果表明,尿样中调环酸钙的质量浓度在0.20~5.00μg/mL范围内线性关系良好(R2=0.999),检出限为0.06μg/mL,定量限为0.19μg/mL,回收率在96.41%~104.94%之间。日内相对标准偏差(RSD)为2.14%~3.89%,日间RSD为5.01%~7.58%。该方法前处理简单可行,适合尿样中调环酸钙的测定。Prohexadion-calcium was purified by Waters Oasis MAX column （3cc） cartridges and determinated by HPLC-UV. The standard curves for prohexadion-calcium showed good linearity in the range of 0.20-5.00 /ag/mL with the correlation coefficient R2 = 0. 999. The recoveries were 96.41%- 104.94%. The relative standard deviations（RSDs） of the interassys were 2. 14%-3.89% and RSDs of intraassays were 5.01%-7.58%, respectively. The detection limit of prohexadion-calcium was 0.06 μg/mL, and the limit of quantification for prohexadion-calcium was 0. 19 μg/mL. This method was simple and suitable for the determination of prohexadion-calcium in urine.

关 键 词：尿样 调环酸钙 固相萃取 高效液相色谱法 

分 类 号：O657.12[理学—分析化学]