| 地表水体中同时分析18种糖皮质激素方法的建立 |
| 摘要点击 2547 全文点击 1298 投稿时间：2014-11-10 修订日期：2015-02-05 |
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| 中文关键词 地表水 糖皮质激素 超高液相色谱串联质谱 固相萃取 内分泌干扰物质 |
| 英文关键词 surface water glucocorticoids ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) solid-phase extraction (SPE) endocrine disrupting chemicals (EDCs) |
| 作者 | 单位 | E-mail | | 郭文景 | 北京林业大学环境科学与工程学院, 北京市污染水体源控制技术重点实验室, 北京 100083
南京师范大学地理科学学院, 南京 210046
中国环境科学研究院, 环境基准与风险评估国家重点实验室, 北京 100012 | gwj1990@163.com | | 常红 | 北京林业大学环境科学与工程学院, 北京市污染水体源控制技术重点实验室, 北京 100083
中国环境科学研究院, 环境基准与风险评估国家重点实验室, 北京 100012 | changh@bjfu.edu.cn | | 孙德智 | 北京林业大学环境科学与工程学院, 北京市污染水体源控制技术重点实验室, 北京 100083 | | | 吴丰昌 | 中国环境科学研究院, 环境基准与风险评估国家重点实验室, 北京 100012 | | | 杨浩 | 南京师范大学地理科学学院, 南京 210046 | |
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| 中文摘要 |
| 建立了一种采用固相萃取-超高效液相色谱串极质谱联用系统(UPLC-MS/MS)同时测定地表水体中18种糖皮质激素的高灵敏分析方法. 样品经过HLB固相萃取柱富集净化、V(乙腈)/V(乙酸乙酯)=1: 1,洗脱后,用UPLC-MS/MS测定. 流动相为甲醇和0.1%乙酸水溶液(体积比),采用梯度洗脱,实现了18种目标物质的基线分离,线性范围为1.0~1000 μg ·L-1. 实际水样的加标回收率为65%~108%. 整个分析的方法检出限(MDL)除醋酸可的松和醋酸氢化可的松为10 ng ·L-1外,其他均在0.10 ng ·L-1和1.0 ng ·L-1之间. 应用此方法于北京地表水体5个样品,检测到8种糖皮质激素,浓度范围0.20~476 ng ·L-1,其中曲安西龙、曲安奈德、醋酸氢化可的松和丙酸氯倍他索在地表水中首次检出,证明了该方法的有效性. |
| 英文摘要 |
| A method of ultra-performance liquid chomatography tandam mass spectrometry(UPLC-MS/MS) combined with solid-phase extraction (SPE) has been developed for simultaneous analysis of 18 glucocorticoids in surface water. The analytes were first enriched and purified through a HLB cartridge, and eluted with acetonitrile/ethyl acetate (1: 1, V/V), then detected by UPLC-MS/MS. The detection used gradient elution process with methanol and 0.1% formic acid/water (V/V) as the mobile phase to achieve baseline separations of these 18 analytes. The linear range was 1.0-1000 μg ·L-1. The method detection limits (MDLs) were 0.10-1.0 ng ·L-1 except for cortisone acetate and cortisol acetate(10 ng ·L-1) with overall mean recoveries of 65%-108% in surface water. Application of this method for 5 surface waters from Beijing area showed that 8 glucocorticoids were detected with the concentration range of 0.20-476 ng ·L-1. Triamcinolone, triamcinolone acetonide, cortisol acetate and clobetasol propionate were detected for the first time in surface water samples, suggesting that this method is efficient for real sample analysis. |
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