Analysis method of solid phase extraction coupling solid phase micro extraction

An analysis method and extraction technology, which is applied in the analysis field of solid-phase extraction coupled with solid-phase microextraction technology, can solve the problems of large sampling volume, high detection limit, and inability to analyze PBDEs in natural water bodies.

Inactive Publication Date: 2010-07-21
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 1. The technical problem to be solved by the invention: the existing PBDEs analysis method in water has a generally high detection limit, and generally cannot realize the analysis of PBDEs in natural water bodies; althoug

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Determination of mass spectrometry conditions

[0025] This method adopts the more advanced triple quadrupole in the analysis of environmental samples, selects 13 kinds of PBDEs secondary mass spectrometry characteristics for qualitative and quantitative analysis, thereby improving the sensitivity and reducing the detection limit. Accurate configuration contains 13 kinds of polybrominated diphenyl ethers (BDE-17, BDE-28, BDE-71, BDE-47, BDE-66, BDE-100, BDE-99, BDE-85, BDE-154, BDE-153, BDE- 138, BDE-183, BDE-190, the concentration is 100ng / mL) standard working solution 1mL. The following work is carried out in three steps. In the first step, set the scantype to full scan, scan mode to ms mode, use Q3MS as the detector, set the ion source temperature to 280°C, the transfer line temperature to 280°C, and use the default settings of the instrument for other settings , sample injection, after obtaining the mass spectrum, select the maximum abundance ion of each compo...

Embodiment 2

[0052] Control of method blanks

[0053] The content of PBDEs in the actual water sample measured by this method is extremely low, and the operation process is easily disturbed by the outside world. The control of method blank is extremely important to the whole process. The whole pre-analysis process includes: water sample passing through the membrane, SPE column enrichment, organic solvent elution SPE column, rotary evaporation, nitrogen blowing and SPME enrichment. Follow the sequence from back to front, step by step to make a blank, looking for possible sources of interference. Finally, it was found that the four steps of water sample passing through the membrane, organic solvent elution SPE column, nitrogen blowing and SPME enrichment did not have the possibility of being contaminated by PBDEs in the laboratory environment. There are problems in the two steps of SPE column enrichment and rotary evaporation. The chromatographic results obtained by blank injection showed...

Embodiment 3

[0056] Environmental sample determination

[0057] In order to cooperate with the National Natural Science Foundation of China's key project "Research on Typical Environmental Processes and Structure-Effect Relationships of Persistent Organic Pollutants", eight water sources in Jiangsu Province were selected (Erdun Bridge in Yangzhong City, Pizhou Water Supply Company, Linjiaba Water intake, Taihu Siqian Village, Peixian Water Supply Company, Qiligou, Wujiang Water Purification Plant, Zhangjiagang City Sanshui Plant) were used as sampling points, and 1 L of water samples were collected each, passed through a 0.45 μm filter membrane, and filtered with n-hexane, dichloromethane, The SPE activated by methanol and water is enriched, and the enrichment speed is controlled at about 10min / min. Put the enriched SPE column on the elution device, use 5ml n-hexane and 10ml 1:1 n-hexane / dichloromethane for elution, collect the eluate in a pear-shaped bottle, rotate it to nearly dryness, a...

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Abstract

The invention discloses an analysis method of solid phase extraction coupling solid phase micro extraction, belonging to the technical filed of analysis methods. The method comprises the following steps: filtering water sample by a filter film; activating an SPE enriching column, and then enriching the water sample; eluting the enriched PBDEs in the SPE enriching column and collecting eluent; distilling collected elution solution and condensing to close to dry; transferring the elution substance into an extraction bottle and drying by nitrogen; putting optical fiber with a polydimethylsiloxane coating at a GC injection port and then activating at 260-300 DEG C; adding methanol and distilled water into the extraction bottle dried by nitrogen and carrying out ultrasound blending to form a water sample to be detected, dipping activated optical fiber in the water sample to be tested for extraction; and drying the extracted optical fiber at the injection port, carrying out GC-MS analysis after thermal desorption. In the invention, solid phase extraction is coupled with solid phase microextraction, thus being suitable for analyzing ultratrace polybrominated diphenyl ethers, having low coat and small workload, in addition, the limit of detection of analyzing PBDEs is between 0.06pg/L and 1.84pg/L.

Description

technical field [0001] The present invention relates to an analysis method of solid-phase extraction coupling solid-phase microextraction technology applied to the analysis of trace organic matter, more specifically a solid-phase extraction coupling solid-phase microextraction method for analyzing ultra-trace polybrominated diphenyl ethers in water analysis method. Background technique [0002] The basic characteristics of persistent organic pollutants (POPs), such as lipophilicity, refractory degradation, and easy accumulation by biological organisms, make humans at the top of the food chain the most vulnerable population. Studies around the world have shown that the content of polybrominated diphenyl ethers (PBDEs) in human tissues and organs continues to increase. Based on this, more and more regulations have banned or restricted the production and use of such substances, for example, pentabrominated and octabrominated Brominated diphenyl ethers were also banned by the E...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 于红霞苏冠勇邬旸温泉韦斯刘红玲
Owner NANJING UNIV
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