干旱区生态环境知识资源中心(Arid): 超高效液相色谱-四极杆串联飞行时间质谱法筛查上海市生活饮用水和地表水中的雌激素水平

Arid

	超高效液相色谱-四极杆串联飞行时间质谱法筛查上海市生活饮用水和地表水中的雌激素水平
其他题名	Screening estrogens in drinking water and surface water of Shanghai city using ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry
	王和兴; 周颖; 王霞; 屈卫东; 姜庆五
来源期刊	复旦学报. 医学版
ISSN	1672-8467
出版年	2011
卷号	38 期号:5 页码:396-401,406
中文摘要	目的建立应用超高效液相色谱-四级杆串联飞行时间质谱法快速筛查上海市生活饮用水和地表水中天然或人工合成的雌激素的方法。方法分别采集上海市不同地点生活饮用水、黄浦江与苏州河不同河段地表水水样各1L，每点设2个平行，取500mL水样经OasisHLB固相萃取柱(500mg，Waters)萃取，70%甲醇淋洗， 10mL体积分数为10%的甲醇乙酸乙酯溶液洗脱待测物，用WatersACQUITYUPLCHSST3色谱柱(100mm* 2.1mm，1.8mum)分离，在MS和MS/MS模式下，采用负离子模式电喷雾离子源对常见雌激素进行Q-TOFMS分析。结果5种常见雌激素(雌三醇、beta-雌二醇、17alpha-乙炔雌二醇、雌酮、己烯雌酚)在0.001～0.1mug/mL范围内线性关系良好，检出限(S/N=3)为0.11～0.25ng/L，定量限(S/N=10)为0.38～0.84ng/L，在添加水平分别为5.50ng/L时，平均回收率为58%～115%，RSD为1.4%～13.9%，5种雌激素测定其相对分子质量(Mr)与理论值的误差在(-1.7～2.8)x10~(-3)之间。生活饮用水中未检出上述5种雌激素，而黄浦江和苏州河的各个河段的水样中均检测出雌三醇(0.8～10.5ng/L)和雌酮(1.6～5.ong/L)。结论本方法灵敏度高、定性准确，适用于生活饮用水和地表水中雌激素的筛查。流经上海市不同河段的黄浦江和苏州河水样中均检测出ng/L级的雌三醇和雌酮，应当在今后的监测中引起重视。
英文摘要	Objective To develop a screening method for natural or synthetic estrogens in drinking water and surface water in Shanghai using ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS).Methods Duplicate 1 L drinking water and surface water samples were obtained from different sites in Shanghai city,Suzhou River and Huangpu River,respectively.The compounds in 500 mL water sample were extracted by Oasis HLB column(500 mg,Waters),washed by 70 % methanol,eluted by the mixture containing 10% methanol in ethyl acetate (volume percentage),and then separated on a Waters ACQUITYUPLC HSS T3 column(100 mm x 2.1 mm,1.8 mum)and analyzed qualitatively and quantitatively by UPLC-Q-TOF in MS and MS/MS model.Results Five frequent estrogens including estriol,beta-estradiol,17a-ethinylestradiol,estrone and diethylstilbestrol had good linearity between 0.001 - 0.1 mug/mL with the limits of detection (LODs)ranging from 0.11 to 0.25 ng/L and the limits of quatitation(LOQs)from 0.38 to 0.84 ng/L.The mass errors between theoretical and experimental masses obtained for deprotonated molecules of five estrogens,internal standard(beta-estradiol-d3)and their daughter ions were between (- 1.7 - 2.8)x 10-3 (Mr).At the spiked levels of 5,50 ng/L,the average recoveries ranged from 58% to 115% with the relative standard deviations between 1.4% and 13.9%.No target estrogens were found in drinking water,but estriol (0.8 - 10.5 ng/L)and estrone (1.6 - 5.6 ng/L)were all detected in surfacewater samples from Suzhou River and Huangpu River.Conclusions The proposed method was sensitive,accurate and suitable for screening estrogens in drinking water and surface water.Estriol and estrone at ng/L level exist in Suzhou River and Huangpu River,which should be paid more attention in further surveillance.
中文关键词	雌激素 ; 生活饮用水 ; 地表水 ; 超高效液相色谱一四极杆串联飞行时间质谱法
英文关键词	estrogens drinking water surface water ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS)
语种	中文
国家	中国
收录类别	CSCD
WOS类目	BIOPHYSICS
WOS研究方向	Biophysics
CSCD记录号	CSCD:4310508
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/226385
作者单位	复旦大学公共卫生学院, 公共卫生安全教育部重点实验室, 上海 200032, 中国
推荐引用方式 GB/T 7714	王和兴,周颖,王霞,等. 超高效液相色谱-四极杆串联飞行时间质谱法筛查上海市生活饮用水和地表水中的雌激素水平[J],2011,38(5):396-401,406.
APA	王和兴,周颖,王霞,屈卫东,&姜庆五.(2011).超高效液相色谱-四极杆串联飞行时间质谱法筛查上海市生活饮用水和地表水中的雌激素水平.复旦学报. 医学版,38(5),396-401,406.
MLA	王和兴,et al."超高效液相色谱-四极杆串联飞行时间质谱法筛查上海市生活饮用水和地表水中的雌激素水平".复旦学报. 医学版 38.5(2011):396-401,406.