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气相色谱-串联质谱法测定木制儿童用品中的10种木材防腐剂
其他题名Determination of 10 Preservatives in Wooden Children’s Products by Gas Chromatography-Tandem Mass Spectrometry
吕庆1; 李海玉1; 李丕1; 李文涛1; 郭项羽1; 王烨1; 白桦1; 齐美玲2; 张庆1
来源期刊质谱学报
ISSN1004-2997
出版年2013
卷号34期号:6页码:321-329
中文摘要建立了固相萃取-气相色谱-串联质谱法(SPE-GC-MS/MS)同时测定木制儿童用品中氯酚类化合物和菊酯类化合物等10种木材防腐剂。采用甲醇溶剂提取,乙酸酐试剂衍生、固相萃取净化后,经HP-5MS色谱柱(30 m*0.25 mm*0.25 mum)分离,串联质谱在多反应离子监测模式(MRM)下进行检测,内标法定量。同时,考察了多种实验参数对检测结果的影响,并进行方法验证。结果表明,该方法对于复杂基质的木材样品中目标物的检测具有良好的选择性与灵敏度。对于不同物质的定量限(LOQ)在0.002 5~0.2 mg/kg之间,线性范围为0.002 5~25 mg/kg,低、中、高3个添加水平的平均回收率在85.2%~100.1%之间,日内精密度(RSD,n=6)在0.6%~9.1%之间,日间精密度(RSD,n=6)在2.3%~7.2%之间。将该方法应用于实际样品抽查中,发现了多种木材防腐剂的残留。
英文摘要Ten kinds of wood preservatives of chlorophenols and pyrethroids in wooden children’s products were determined simultaneously using solid phase extraction coupled with gas chromatography-tandem mass spectrometry (SPE-GC-MS/MS). The sample was ultrasonically extracted with methanol. The extract was evaporated and then derivatised with acetic anhydride. Finally the solution was purified using Oasis HLB SPE column. The separations were performed on an Agilent HP-5MS column (30 m*0.25 mm*0.25 mum), then were determined by MS/MS and quantified by internal standard method. Procedures for extraction and purification were carefully optimized. The method was proved to be linear over a wide range of concentrations for all analytes with the correlation coefficients greater than 0.999 3. Limits of detection (LODs) and limits of quantification (LOQs) are in the range of 0.0010.05 mg/kg and 0.002 50.2 mg/kg, respectively. Average recoveries of target compounds (spiked at three concentration levels) are in the range of 85.2%100.1%. Intraday and interday repeatability (RSD, n=6) of the proposed method are vary of 0.6%9.1% and 2.3%7.2%, respectively. The proposed method was used to monitor preservatives in commercial wooden toys, and some preservatives were found.
中文关键词气相色谱-串联质谱法 ; 木材防腐剂 ; 固相萃取 ; 木制儿童用品
英文关键词gas chromatography-tandem mass spectrometry wood preservatives solid phase extraction wooden children’s products
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:4993052
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/230466
作者单位1.中国检验检疫科学研究院,工业与消费品安全研究所, 北京 100123, 中国;
2.北京理工大学化学学院, 北京 100081, 中国
推荐引用方式
GB/T 7714
吕庆,李海玉,李丕,等. 气相色谱-串联质谱法测定木制儿童用品中的10种木材防腐剂[J],2013,34(6):321-329.
APA 吕庆.,李海玉.,李丕.,李文涛.,郭项羽.,...&张庆.(2013).气相色谱-串联质谱法测定木制儿童用品中的10种木材防腐剂.质谱学报,34(6),321-329.
MLA 吕庆,et al."气相色谱-串联质谱法测定木制儿童用品中的10种木材防腐剂".质谱学报 34.6(2013):321-329.
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