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大体积进样/气相色谱-质谱联用(PTV/GC-MS)快速分析水体中痕量缓蚀剂 | |
其他题名 | Simultaneous Determination of Trace Benzotriazoles and Benzothiazoles in Water by Large-volume Injection/Gas Chromatography-Mass Spectrometry |
刘芳文; 颜文; 徐维海 | |
来源期刊 | 分析测试学报
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ISSN | 1004-4957 |
出版年 | 2015 |
卷号 | 34期号:3页码:341-345 |
中文摘要 | 建立了水体中12种缓蚀剂(苯并噻唑和苯并三唑类衍生物)的大体积进样/气相色谱-质谱联用(PTV/GC-MS)的高灵敏度分析方法。1. 0 L 水样经0. 45 mum 滤膜过滤后调至pH 3. 0,通过HLB 固相萃取柱富集。目标化合物经6 mL 甲醇-乙腈(1 ∶ 1)淋洗,洗脱液用氮气吹扫至近干后,加入丙酮、内标物和硅烷化试剂定容至1 mL,置于烘箱中38 ℃衍生化1 h 后,密封于细胞瓶中待测。试样采用DB-5MS 气相色谱柱进行分离,选择离子模式(SIM)测定。结果表明,目标化合物在0. 1 ~ 100 ng/L 质量浓度范围内呈良好线性,相关系数均不小于0. 992。自来水中12种化合物的平均加标回收率为46%~ 116%,相对标准偏差(RSD)为1. 0%~ 16%。河水中目标化合物的回收率为43%~ 117%,RSD 为1. 0%~ 15%。自来水和河水中目标化合物的检出限分别为0. 050 ~ 1. 3 ng/L 和0. 057 ~ 1. 8 ng/L。该方法成功用于广州珠江河段缓蚀剂污染物含量的分析。 |
英文摘要 | A rapid and reliable analytical method,based on large-volume injection and gas chromatography-mass spectrometry (PTV/GC-MS)was developed for the determination of 12 benzotriazoles and benzothiazoles in aquatic matrixes. 1. 0 L water samples were acidified to pH 3. 0 using 3 mol/L HCl. The samples were then passed through an Oasis HLB cartridge. The analytes were eluted with 6 mL methanol-acetonitrile(1 ∶ 1). The solution was evaporated to dryness under a gentle stream of nitrogen,and redissolved in acetone,internal standard and silylation reagent. The sealed vials were incubated at 38 ℃ for 1 h before instrument analysis. The separation of target compounds was achieved in a DB-5MS fused-silica capillary column. The analytes were detected in selected ion monitoring(SIM)that operated in electron impact(EI)mode. The calibration curves of 12 target compounds were linear in the range of 0. 1-100 ng/L with correlation coefficients not less than 0. 992. Spiked recoveries of the target analytes were in the ranges of 46%-116% for tap water,and 43%-117% for river water,with RSDs of 1. 0%-16% and 1. 0%-15%,respectively. The method detection limits for tap water and river water were in the ranges of 0. 050-1. 3 ng/L and 0. 057-1. 8 ng/L,respectively. The method was simple and sensitive,and was successfully employed in the detection of corrosion inhibitors in river water collected from the city section of the Pearl River. |
中文关键词 | 缓蚀剂 ; 固相萃取 ; 硅烷化 ; 气相色谱-质谱联用 ; 河水 |
英文关键词 | corrosion inhibitor solid phase extraction silylation gas chromatography-mass spectrometry(GC-MS) river water |
语种 | 中文 |
国家 | 中国 |
收录类别 | CSCD |
WOS类目 | CHEMISTRY ANALYTICAL ; ENGINEERING CHEMICAL |
WOS研究方向 | Chemistry ; Engineering |
CSCD记录号 | CSCD:5395775 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/232581 |
作者单位 | 中国科学院南海海洋研究所, 广州, 广东 510301, 中国 |
推荐引用方式 GB/T 7714 | 刘芳文,颜文,徐维海. 大体积进样/气相色谱-质谱联用(PTV/GC-MS)快速分析水体中痕量缓蚀剂[J],2015,34(3):341-345. |
APA | 刘芳文,颜文,&徐维海.(2015).大体积进样/气相色谱-质谱联用(PTV/GC-MS)快速分析水体中痕量缓蚀剂.分析测试学报,34(3),341-345. |
MLA | 刘芳文,et al."大体积进样/气相色谱-质谱联用(PTV/GC-MS)快速分析水体中痕量缓蚀剂".分析测试学报 34.3(2015):341-345. |
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