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Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples

A complex sample and selective technology, applied in the field of selective separation, to achieve good separation effect, high separation efficiency and simple operation

Active Publication Date: 2013-10-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the selective separation of PCN, HBCD and TBBPA has not been reported

Method used

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  • Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples
  • Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples
  • Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 8 g of silica gel was packed tightly into a chromatographic column (outer diameter 26 mm, length 305 mm), and a vacuum pump was used to pump the filler tightly. Before loading the sample, use 50mL n-hexane to activate the chromatography column; then mix 1mL polychlorinated naphthalene, hexabromocyclododecane and tetrabromobisphenol A with the -1 , Hexabromocyclododecane 500ng mL -1 , Tetrabromobisphenol A 500ng mL -1 , and the rest is n-hexane solvent) for sample loading. After the sample was loaded, 200 mL of n-hexane, 200 mL of n-hexane and dichloromethane mixed solvent (volume ratio 1:1), and 4×50 mL of dichloromethane were used for elution to obtain six different eluents. The six groups of eluents were rotary evaporated to constant volume, and then analyzed by gas chromatography tandem mass spectrometry or high performance liquid chromatography tandem mass spectrometry.

[0023] From figure 1 It can be seen that when silica gel is used as the chromatography colu...

Embodiment 2

[0025] 8g of 3% deactivated silica gel (the mass ratio of deionized water and silica gel is 3: 100 is used to mix, and the deactivation process is carried out) is tightly packed in the chromatographic column (26mm in outer diameter, 305mm in length), and uses a vacuum pump to The filling is firm. Before loading the sample, use 50mL n-hexane to activate the chromatography column; then mix 1mL polychlorinated naphthalene, hexabromocyclododecane and tetrabromobisphenol A with the -1 , Hexabromocyclododecane 500ng mL -1 , Tetrabromobisphenol A 500ng mL -1 , and the rest is n-hexane solvent) for sample loading. After loading the sample, use 100mL n-hexane, 2×50mL n-hexane and dichloromethane mixed solvent (volume ratio 1:1), 2×50mL n-hexane and dichloromethane mixed solvent (volume ratio 1:3) and 2× 50mL of dichloromethane was used for elution, and seven groups of different eluents were obtained. The seven groups of eluents were rotary evaporated to constant volume, and then an...

Embodiment 3

[0028] First, 10 g of soil was extracted by the Soxhlet extraction method (the extraction solvent was a mixed solvent of n-hexane and dichloromethane with a volume ratio of 250 mL of 1:1), and then the extract containing the target analyte was concentrated by rotary evaporation until it was concentrated to After about 500 μL, rinse the flat-bottomed flask with n-hexane three times, then transfer the eluent to a test tube and dilute to 10 mL.

[0029] 8g of 3% deactivated silica gel (the mass ratio of deionized water and silica gel is 3: 100 is used to mix, and the deactivation process is carried out) is tightly packed in the chromatographic column (26mm in outer diameter, 305mm in length), and uses a vacuum pump to The filling is firm. Before loading the sample, use 50mL n-hexane to activate the chromatographic column; then add polychlorinated naphthalene, hexabromocyclododecane and tetrabromobisphenol A mixed standard to 1mL (polychlorinated naphthalene 100ngmL -1 , Hexabrom...

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Abstract

The invention relates to utilization of a silica matrix as a sample pretreatment material, wherein a) PCNs (polychlorinated naphthalenes congeners), HBCDs (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples are extracted by a solvent extraction method and an extract containing target analytes is obtained; b) the silica matrix is selected as a chromatographic column filler; the filer is activated by using normal hexane at first and then the extract is loaded; c) the polychlorinated naphthalenes congeners, hexabromocyclododecanes and tetrabromobisphenol A are eluted orderly by using organic solvents (normal hexane, dichloromethane and the like) composed of different solvents, and then three eluates of different fractions are obtained; d) after solvents are volatilized from the eluates, the purified target analytes are obtained. According to the invention, selective separation of the polychlorinated naphthalenes congeners, hexabromocyclododecanes and tetrabromobisphenol A in the complex samples is realized by virtue of a simple chromatographic column; the method has the advantages of simplicity in operation, good selectivity and high efficiency.

Description

technical field [0001] The present invention relates to the selective separation method of polychlorinated naphthalene (PCNs), hexabromocyclododecane (HBCDs) and tetrabromobisphenol A (TBBPA) in complicated sample, specifically a kind of using silica gel substrate as chromatographic column Packing, a method for selectively separating three types of substances in sediment, soil and biological samples. Background technique [0002] Commercial hexabromocyclododecane is commonly used in polystyrene foam. Due to its high yield and the characteristics of persistent organic pollutants, it is defined by the European Chemicals Agency as a priority pollutant and a high-volume chemical. Tetrabromobisphenol A is a reactive brominated flame retardant, commonly used in circuit boards, and is currently the most widely used flame retardant product. As one of the ubiquitous organic pollutants, it has been detected in many environmental media. Polychlorinated naphthalenes can be transmitted...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 金静縢曼陈吉平倪余文田玉增王龙星
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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