干旱区生态环境知识资源中心(Arid): 气相色谱-质谱法测定生物检材中水胺硫膦

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	气相色谱-质谱法测定生物检材中水胺硫膦
其他题名	Determination of Isocarbophos in Bio-testing Materials by GC-MS
	王云玉 1; 蔡明招 1; 吴惠勤 2; 朱志鑫 2
ISSN	1001-4020
出版年	2009
卷号	45 期号:4 页码:437-439
中文摘要	PH 4.5生物检材溶液中的水胺硫膦用Oasis HLB 3cc固相萃取小柱分离,此小柱经离心干燥后用乙酸乙酯淋洗,所得洗出液吹氮浓缩至1 mL供气相色谱-质谱法(GC-MS)分析用,对GC-MS分析的条件进行了试验并给出了优化的分析参数.为了避免和减少样品的热分解,方法中采用了较高的柱前压,较高的载气流量以及较低的GCMS间的接口温度.根据水胺硫膦标准的质谱图,确定了各主要强离子碎片的归属,并提出了水胺硫膦的标准谱库,作为水胺硫膦定性分析的基础.测定水胺硫膦的线性范围在0.05～100 mg·L~(-1)之间,试验测得方法的平均回收率、相对标准偏差(n=5)及检出限(3S/N)依次为93.3%,2.5%及0.05 mg·L~(-1).
英文摘要	Isocarbophos in bio-testing materials was separated by SPE on Oasis HLB SPE column from sample solution buffered at pH 4. 5 with PBS. The SPE column was dried by centrifugation and eluted with ethylacetate to desorb isocarbophos from the column. The eluate was concentrated to 1 mL by N_2 -blowing and used for GC-MS analysis. Conditions for GC-MS analysis ware studied and the optimum parameters were given. Relatively high pre-column pressure, high flow-rate of carrying gas and low temperature at the connection inlet from GC to MS were adopted to reduce or avoid thermodecomposition of sample. Based on the mass spectrogram of standard isocarbophos, the attribution of strong ion fragments were confirmed and standard spectrum database of isocarbophos was proposed, which is the basis of qualitative analysis of isocarbophos. Range of linearity found for determination of isocarbophos was between 0. 05-100 mg·L~(-1). Values of average recovery, RSD (n=5) and limit of detection (3S/N) were found to be 93. 3%, 2. 5% and 0. 05 mg·L~(-1) respectively.
中文关键词	固相萃取法 ; 气相色谱-质谱联用 ; 水胺硫膦 ; 生物检材
英文关键词	Solid-phase extraction (SPE) GC-MS Isocarbophos Bio-testing materials
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:3601309
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/223905
作者单位	1.华南理工大学,化学科学学院, 广州, 广东 510640, 中国; 2.中国广州分析测试中心, 广东省化学危害应急检测技术重点实验室, 广州, 广东 510070, 中国
推荐引用方式 GB/T 7714	王云玉,蔡明招,吴惠勤,等. 气相色谱-质谱法测定生物检材中水胺硫膦[J],2009,45(4):437-439.
APA	王云玉,蔡明招,吴惠勤,&朱志鑫.(2009).气相色谱-质谱法测定生物检材中水胺硫膦.,45(4),437-439.
MLA	王云玉,et al."气相色谱-质谱法测定生物检材中水胺硫膦".45.4(2009):437-439.