干旱区生态环境知识资源中心(Arid): 液相色谱串联质谱法定量检测尿中有机磷农药代谢物

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	液相色谱串联质谱法定量检测尿中有机磷农药代谢物
其他题名	Method establishment for the determination of 6 organophosphorus pesticides metabolites in human urine using LC-MS/MS
	周志荣; 张淼; 林少彬
来源期刊	卫生研究
ISSN	1000-8020
出版年	2013
卷号	42 期号:1 页码:122-126
中文摘要	目的建立了液相色谱串联质谱(LC-MS/MS)法测定尿中二乙基磷酸酯、二硫代磷酸二甲酯、二硫代磷酸二乙酯、4-硝基酚、3-氯-4-甲基-7-羟基香豆素和TCPY 6种有机磷农药代谢物含量的方法。方法尿样中加入酶解液, 37℃水浴4h后经oasis HLB柱固相萃取, 用甲醇洗脱后离心浓缩, 乙腈定容;以乙酸铵做缓冲溶液, 乙腈和水为流动相等梯度洗脱, 经Waters Symmetry C_(18) 5mum(2.1mm*150mmcolumn)分离, 经在线电喷雾离子源(ESI)负离子化后, 采用多反应离子监测方式(MRM)选择离子对测定。结果目标化合物的线性范围为0~1000ng/ml, 6种化合物的相关系数有5种大于0.990, 加标回收率在79%~130%之间, RSD<8.2%;日内、日间相对标准偏差小于15%(n=6)。结论该方法样品采集简单, 特异性强, 能准确、高效地检测尿样中有机磷农药代谢物。
英文摘要	Objective To establish a method to determine the presence and concentration of DEP,DMDTP,DEDTP,PNP,CMHC and TCPY organophosphorus pesticides metabolites in human urine by LC-MS /MS. Method 2. 0ml of urine was enzymatically hydrolyzed in water bath 37℃ for 4 hours, then the urine samples were solid-phase extracted by Oasis HLB and eluted with methanol,after centrifugation and concentration the urine samples were separated on waters symmetry C_(18) 5mum(2. 1mm #150mm) column with ammonium acetate buffer solution acetonitrile-water as mobile phase to constant gradient elution. Electrospray ionization source (ESI) was applied and operated in positive ion mode,and multiple reaction monitoring (MRM) mode was adopted. Results Within concentration ranging from 0 - 1000ng /ml the correlation coefficient for 5 compounds of 6 were greater than 0. 990,recoveries were between 79%-130%, RSD < 8. 2%. The RSD of intra-day and inter-day were less than 15% (n = 6). Conclusion The procedure of samples collection is simple. This is a accurate and specific method for testing organophosphorus pesticides metabolites in human urine.
中文关键词	液相色谱串联质谱 ; 有机磷农药代谢物 ; 尿样 ; 固相萃取
英文关键词	LC-MS /MS organophosphorus pesticides metabolites urine solidphase extraction
语种	中文
国家	中国
收录类别	CSCD
WOS类目	PUBLIC ENVIRONMENTAL OCCUPATIONAL HEALTH
WOS研究方向	Public, Environmental & Occupational Health
CSCD记录号	CSCD:4788083
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/230266
作者单位	中国疾病预防控制中心环境与健康相关产品安全所, 北京 100021, 中国
推荐引用方式 GB/T 7714	周志荣,张淼,林少彬. 液相色谱串联质谱法定量检测尿中有机磷农药代谢物[J],2013,42(1):122-126.
APA	周志荣,张淼,&林少彬.(2013).液相色谱串联质谱法定量检测尿中有机磷农药代谢物.卫生研究,42(1),122-126.
MLA	周志荣,et al."液相色谱串联质谱法定量检测尿中有机磷农药代谢物".卫生研究 42.1(2013):122-126.