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Isotope dilution high resolution chromaticness combination method for simultaneously detecting organic chlorine pesticides and polychlorinated biphenyl in biological sample, and application

A technology for polychlorinated biphenyls and biological samples, applied in the field of environmental analysis, can solve the problems of inability to pre-treatment and simultaneous detection of organochlorine pesticides and polychlorinated biphenyls

Inactive Publication Date: 2016-07-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The U.S. EPA has promulgated high-resolution mass spectrometry analysis methods for the detection of organochlorine pesticides (EPA1699-2007) and polychlorinated biphenyls (EPA1668B-2008), but the pretreatment and detection methods of organochlorine pesticides and PCBs belong to the Different method systems are two completely different methods. The high-resolution mass spectrometry method promulgated by the EPA cannot simultaneously perform sample pretreatment and simultaneous detection of organochlorine pesticides and PCBs.

Method used

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  • Isotope dilution high resolution chromaticness combination method for simultaneously detecting organic chlorine pesticides and polychlorinated biphenyl in biological sample, and application
  • Isotope dilution high resolution chromaticness combination method for simultaneously detecting organic chlorine pesticides and polychlorinated biphenyl in biological sample, and application
  • Isotope dilution high resolution chromaticness combination method for simultaneously detecting organic chlorine pesticides and polychlorinated biphenyl in biological sample, and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1. Sample pretreatment and extraction with internal standard extraction

[0016] This method is applicable to all biological samples. Taking the biological sample mussel as an example to illustrate the sample pretreatment. A proper amount of mussel samples was collected, after washing and shelling, the mussel tissue and slurry were homogenized together, and then vacuum freeze-dried at a low temperature of -40°C. The dried mussel samples were pulverized with a pulverizer and passed through a 120-mesh sieve to obtain a mussel dry powder sample, and the above samples were thoroughly mixed.

[0017] Weigh 2.00g of mussel sample and add 13 10 μl of C-labeled 6 kinds of indicative internal standards for PCB extraction (label P48MES, concentration 120ppb, namely 28, 52, 101, 138, 153, 180), 13 10 μl of C-labeled 12 kinds of toxic PCB extraction internal standards stipulated by WHO (P48WES, concentration 100ppb, namely 81, 77, 123, 118, 114, 105, 126, 167, 156, 157, ...

Embodiment 2

[0020] Example 2. Gel Permeation Chromatography (GPC) Cleanup

[0021] Use 1:1 n-hexane and dichloromethane as mobile phase, flow rate 5mL / min, use GPC calibration solution (containing 2.5mg / mL corn oil, 0.05mg / mL bis(2-ethylhexyl)phthalic acid Esters (BEHP, 0.01mg / mL methoxychlor, 0.002mg / mL perylene, 0.008mg / mL sulfur) corrected the fraction collection time of gel permeation chromatography, that is, the junction of the two peaks of phthalate and methoxychlor The bottom of the valley is used as the starting point for collecting fractions, and the bottom of the valley where the two peaks of perylene and sulfur meet is used as the end point of collecting fractions. After the extract in Example 1 was concentrated to about 1.5mL, it was first passed through a 0.45μm filter membrane, and then passed through a GPC column (450mm×25mm, filled with 75g of SX-3Bio-beads) for purification, and the GPC calibration solution was collected The fraction of the corrected time period (here, t...

Embodiment 3

[0022] Embodiment 3. Fluorisil column purification or silica gel column purification

[0023] Concentrate the fraction collected in Example 2 to about 1-2 mL, and purify it through a florisil column (a glass column with an inner diameter of 20 mm x a length of 400 mm is filled with 7.6 g of florisil fillers with a particle size of 60-100 mesh). , with 100 mL of a mixed solution of n-hexane and dichloromethane (volume ratio 50:50) to rinse and collect fractions.

[0024] The following method can also be used: Concentrate the fraction collected in Example 2 to about 1-2 mL, pass through a silica gel column (a glass column with an inner diameter of 20 mm x a length of 400 mm is filled with 6.0 g of ordinary silica gel packing with a particle size of 60-100 mesh), The collected fractions were rinsed with 50 mL of a mixed solution of n-hexane and dichloromethane (volume ratio 3:7).

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Abstract

The invention relates to an isotope dilution high resolution chromaticness combination method for simultaneously detecting organic chlorine pesticides and polychlorinated biphenyl in a biological sample. The method can realize simultaneous purification of the two targets of the organic chlorine pesticides and the polychlorinated biphenyl in a pre-treatment process, and a detection process can be carried out simultaneously. The sample pretreatment employs a method combining gel permeation chromatography with Florisil silica column (or silica gel column) purification. A gold standard method using an isotope dilution high resolution GC-MS is employed for the detection. Compared with a traditional low resolution mass spectrum and an electron capture detector (ECD) method, the interference and false positive results are reduced, and the indexes such as the method deletion limit and the quantitative result accuracy are greatly improved. The method can save more than 50% of labour amount, time and consumables such as solvents, and filler materials in comparison with a method for respective and step by step measurement of the organic chlorine and the polychlorinated biphenyl, and has important meaning for research and monitor of the organic chlorine pesticides and the polychlorinated biphenyl.

Description

technical field [0001] The invention relates to the field of environmental analysis, in particular to an isotope dilution high-resolution chromatography-mass method for simultaneously detecting organochlorine pesticides and polychlorinated biphenyls in biological samples and its application. Background technique [0002] Persistent organochlorine pesticides such as polychlorinated biphenyls, BHC, and DDT are persistent organic pollutants stipulated by the Stockholm Convention, and they are pollutants that countries should focus on when implementing the Convention. From home and abroad, the detection of PCBs and organochlorine pesticides POPs pollutants is still based on gas chromatography-electron capture detector (GC-ECD), gas chromatography-low resolution mass spectrometry (GC-LRMS) and other methods. The mainstream technology, the above method is easy to introduce interference, which will bring false positive results and affect the accuracy of the measurement results. As...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 卢宪波陈吉平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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