Nam Vu-Duc, Thuy Minh-Le, Xuyen Nguyen-Thi, Cam Tu Vu, Van-Hoi Bui, Hong An Vu-Thi, Dinh Binh Chu
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引用次数: 0
摘要
摘要采用气相色谱-串联质谱联用技术对污染土壤中的持久性有机污染物有机氯农药进行了分析。以二氯甲烷和正己烷为溶剂,采用加速溶剂萃取法,在高温高压条件下提取ocp。萃取剂经旋转真空蒸发器浓缩,硅胶固相萃取净化。然后用气相色谱法结合电子冲击电离质谱法在质谱/质谱模式下分离OCPs。对GC-EI-MS/MS分析方法的检出限、定量限及重复性、回收率等重要参数进行了研究。检测限和定量限分别为0.005 ~ 0.405 ng g−1 (p,p′-DDE)和0.016 ng g−1 ~ 1.216 ng g−1。该方法短期和长期稳定性的重复性分别低于8.3%和13.7%。所有ocp的回收率为78.1%±1.5% ~ 117.5%±3.2%。在实际样品中进行了峰化实验,验证了所建立的分析方法。该验证方法随后被用于分析从越南污染地区收集的土壤样品中的ocp。结果显示,六氯环己烷异构体和p-p ' -滴滴涕在所有分析样本中均处于较高水平。关键词:有机氯农药;气相色谱-质谱联用/质谱联用污染土壤样品;加速溶剂萃取-硅胶净化;本研究由国家科学技术发展基金资助,批准号[104.04-2018.331]。
Analysis of organochlorine pesticides in contaminated soil by GC-MS/MS using accelerated solvent extraction as a green sample preparation
ABSTRACTOrganochlorine pesticides (OCPs), persistent organic pollutants, in the contaminated soil have been analysed by a gas chromatography-tandem mass spectrometry (MS) in this work. OCPs were extracted with a mixture of dichloromethane and n-hexane by using accelerated solvent extraction at elevated temperature and high pressure. The extractant was concentrated by a rotary vacuum evaporator and cleaned up by silica gel solid phase extraction. OCPs were then separated by a gas chromatography in combination with an electron impact ionisation MS in MS/MS mode. The limit of detection, limit of quantification and other important parameters of the GC-EI-MS/MS analytical method, such as repeatability, recovery and so on, have been investigated and presented. Limit of detection and limit of quantification have been achieved from 0.005 ng g−1 (p,p’-DDE) to 0.405 ng g−1 (dieldrin) and 0.016 ng g−1 to 1.216 ng g−1, respectively. The repeatability of this method was achieved below 8.3% and 13.7% for short- and long-term stability. Recovery of all OCPs ranged from 78.1% ± 1.5% to 117.5% ± 3.2%. The developed analytical method was validated by spiking experiments in the real samples. The validated method has been then used for the analysis of OCPs in the soil samples that were collected from the contaminated areas in Vietnam. Results showed the presence of hexachlorocyclohexane isomers and p-p’-DDT in all analysed samples at elevated levels.KEYWORDS: Organochlorine pesticidesGC-MS/MScontaminated soil samplesaccelerated solvent extractionsilica gel clean-up Disclosure statementNo potential conflict of interest was reported by the author(s).Additional informationFundingThis research is funded by the National Foundation for Science and Technology Development (Nafosted) under the grant number [104.04-2018.331].
期刊介绍:
International Journal of Environmental Analytical Chemistry comprises original research on all aspects of analytical work related to environmental problems. This includes analysis of organic, inorganic and radioactive pollutants in air, water, sediments and biota; and determination of harmful substances, including analytical methods for the investigation of chemical or metabolic breakdown patterns in the environment and in biological samples.
The journal also covers the development of new analytical methods or improvement of existing ones useful for the control and investigation of pollutants or trace amounts of naturally occurring active chemicals in all environmental compartments. Development, modification and automation of instruments and techniques with potential in environment sciences are also part of the journal.
Case studies are also considered, particularly for areas where information is scarce or lacking, providing that reported data is significant and representative, either spatially or temporally, and quality assured. Owing to the interdisciplinary nature of this journal, it will also include topics of interest to researchers in the fields of medical science (health sciences), toxicology, forensic sciences, oceanography, food sciences, biological sciences and other fields that, in one way or another, contribute to the knowledge of our environment and have to make use of analytical chemistry for this purpose.