干旱区生态环境知识资源中心(Arid): 气相色谱/质谱法测定水和沉积物中雄激素与孕激素

Arid

	气相色谱/质谱法测定水和沉积物中雄激素与孕激素
其他题名	Simultaneous Determination of Androgens and Progestogen in Surface Water and Sediment by Gas Chromatography-Mass Spectrometry
	金伟; 黄斌; 王彬; 王道玮; 赵世民; 潘学军
来源期刊	分析化学
ISSN	0253-3820
出版年	2013
卷号	41 期号:2 页码:205-209
中文摘要	建立了气相色谱/质谱联用(GC-MS)技术同时测定水和沉积物中雄激素二氢睾酮、睾丸激素、雄烯二酮和孕激素孕酮的分析方法。分别确定了沉积物微波辅助萃取条件(萃取溶剂、萃取温度和萃取时间)和水样固相萃取条件(固相萃取柱、洗脱溶剂和水样pH值)。结果表明:微波辅助萃取最优条件是乙酸乙酯为萃取溶剂,在120℃萃取15 min;以Oasis HLB为固相萃取柱,水样调节至pH 4,采用乙酸乙酯为洗脱溶剂,固相萃取效果佳。以三甲基碘硅烷为催化剂,N-甲基-N-三甲基硅基三氟乙酰胺为衍生化试剂,将目标化合物分子结构上的羟基和酮基同步衍生化,并确定了衍生化过程的最佳反应温度为40℃,反应时间为20 min,满足了GC-MS分析该类物质的要求。水和沉积物中4种目标化合物检出限分别为0.1~0.5 ng/L和0.6~0.8ng/g,定量限分别为0.4~1.8 ng/L和1.9~2.6 ng/g,加标回收率分别为89.3%~101.4%和77.3%~92.1%,相对标准偏差(RSD)均小于9%。采用本方法对洱海水和沉积物样品进行了分析。
英文摘要	A method based on gas chromatography-mass spectrometry (GC-MS) was established for the simultaneous determination of androgens and progestogen, such as dihydrotestosterone, testosterone, androstenedione and progesterone in surface water and sediment. The method was developed by using microwave-assisted extraction (MAE), solid phase extraction (SPE) and derivatization procedure. The MAE, SPE and derivatization procedure were studied and optimized. The optimized conditions were as follows: using ethyl acetate as extraction solvent, sediment samples were extracted by microwave extraction system at 120 ℃ for 15 min; good recoveries of target compounds were obtained when water samples pH value were adjusted to 4 and Oasis HLB cartridges were used, while ethyl acetate was used as eluting solvent; using trimethyliodosilane as catalytic agent and N-methyl-N-(trimethylsilyl)-trifluoroacetamide as the reagent of derivatization, hydroxyl and ketone groups of target compounds were simultaneous derivatizated at 40 ℃ for 20 min. The method achieved good repeatability and reproducibility with relative standard deviations <9% for all target compounds in both matrices. The recoveries of spiked water and sediment samples were 89.3%-101.4% and 77.3%-92.1%, respectively. The method detection limits for four analytes in sediment samples and water samples were 0.1-0.5 ng/L and 0.6-0.8 ng/L, respectively. The limits of quantification were 0.4-1.8 ng/L and 1.9-2.6 ng/g dry weight (dw) for water samples and sediment samples, respectively. The established method was successfully applied in the determination of target hormones in surface water and sediment samples collected from Erhai Lake, China.
中文关键词	雄激素 ; 孕激素 ; 水 ; 沉积物 ; 气相色谱-质谱联用
英文关键词	Androgens Progestogens Surface water Surface sediment Gas chromatography-mass spectrometry
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:4768931
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/229452
作者单位	昆明理工大学环境科学与工程学院, 昆明, 云南 650500, 中国
推荐引用方式 GB/T 7714	金伟,黄斌,王彬,等. 气相色谱/质谱法测定水和沉积物中雄激素与孕激素[J],2013,41(2):205-209.
APA	金伟,黄斌,王彬,王道玮,赵世民,&潘学军.(2013).气相色谱/质谱法测定水和沉积物中雄激素与孕激素.分析化学,41(2),205-209.
MLA	金伟,et al."气相色谱/质谱法测定水和沉积物中雄激素与孕激素".分析化学 41.2(2013):205-209.