Ultra trace analysis of 17 organochlorine pesticides in water samples from the Arctic based on the combination of solid-phase extraction and headspace solid-phase microextraction-gas chromatography-electron-capture detector
Ultra trace analysis of 17 organochlorine pesticides in water samples from the Arctic based on the combination of solid-phase extraction and headspace solid-phase microextraction-gas chromatography-electron-capture detector
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基于固相萃取与顶空固相微萃取-气相色谱-电子捕获检测器相结合的北极水样中17种有机氯农药的超痕量分析
DOI：
10.1016/j.chroma.2009.12.027
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发表时间：
2010-02-19
影响因子：
4.1
通讯作者：
Cai, Minggang
中科院分区：
文献类型：
--
作者：
Qiu, Canrong;Cai, Minggang
将固相萃取（SPE）与顶空固相微萃取（HS-SPME）相结合，对水样中17种超痕量有机氯农药进行了高效富集。I IS-SPME和SPME纤维的热解吸参数。包括SPE步骤中的洗脱体积和穿透体积、溶剂转化步骤中的温度。纤维类型。离子强度、萃取温度E。通过单因素对比实验和正交实验设计方法对固相微萃取步骤中的萃取时间、萃取温度、萃取时间和萃取温度进行优化，提高了方法的pet。该方法具有较高的灵敏度，方法检出限为0.0018 ~ 0.027 ng L-1。结果表明，该方法具有良好的重复性，相对标准偏差小于20%（IT =4），回收率大于60%，线性范围为00010 ~ 60 ng/mL，R-2值为09988 ~ 09999。该方法成功地应用于北极样品。结果表明，在所有有机氯农药中，六氯环己烷（HCHs）在北极SLIT面水体中的含量最高，SLIM的浓度范围为0 262 ~ 3 156 ng L-1（C）2009 Elsevier B V All rights reserved
Solid-phase extraction (SPE) was combined with headspace solid-phase microextraction (HS-SPME) for the highly effective enrichment of 17 ultra trace organochlorme pesticides in water samples The [at-get compounds were successfully transferred from water samples to a gas chromatography capillary column by means of four consecutive steps, namely SPE, solvent conversion. I IS-SPME, and thermal desorption of the SPME fiber Parameters. including elution volume and breakthrough volume in the SPE step, temperature in the solvent conversion step. and fiber type. ionic strength, extraction temperature e. extraction time, and phi in the SPME step were optimized to Improve the pet of the method through either single factor comparative experiment or the orthogonal experimental design approach After optimization. the method gave high sensitivity with a method detection limit ranging from 0 0018 to 0027 ng L-1. good repeatability with a relative standard deviation less than 20% (IT =4) and acceptable recovery with a value mostly exceeding 60% External standard calibration was employed for the quantification, and a wide linear range (from 00010 to 60ng mL(-1)) with R-2 values ranging from 09988 to 09999 were observed In the end. the method was successfully applied to the Arctic samples. and the results showed that, among all the organochlorine pesticides, hexachlorocyclohexanes (HCHs) were the most predominant in the Arctic SLIT face water body with SLIM of their concentrations ranging from 0 262 to 3 156 ng L-1 (C) 2009 Elsevier B V All rights reserved