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Dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of phthalic acid ester environmental hormone in marine sediment

A technology of phthalate and phthalic acid, which is applied in the field of dispersive solid-phase extraction-gas chromatography-mass spectrometry detection of phthalate environmental hormones, can solve the problem of low recovery rate and can not meet the requirements of analysis and detection and other problems to achieve the effect of accurate results, high sensitivity and simple operation

Active Publication Date: 2018-05-08
MARINE FISHERIES RES INST OF ZHEJIANG
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Problems solved by technology

However, the recovery rate of concentrated sulfuric acid purification method is low. Dispersion liquid-liquid microextraction is mainly suitable for simple liquid matrix samples. For complex solid matrices, it needs to be processed and converted into liquid matrix, and matrix effects are easy to occur.
Zhang Yu et al. used microwave-assisted extraction, C18 adsorbent dispersive solid-phase extraction purification, and gas chromatography-mass spectrometry to determine the phthalates in the soil. The pretreatment of this method needs to add Florisil to the soil sample, matrix effect Obviously, and the adsorbent is only dispersed in the acetone solution, and further research found that C18 in acetone has strong adsorption to dimethyl phthalate and diethyl phthalate, which cannot meet the analysis and detection requirements

Method used

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  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of phthalic acid ester environmental hormone in marine sediment
  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of phthalic acid ester environmental hormone in marine sediment
  • Dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of phthalic acid ester environmental hormone in marine sediment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Determination of 16 kinds of polyphthalates in sediment samples collected at sampling point A of Hangzhou Bay (Beilun District, Zhenhai District) in Ningbo:

[0054] (1) Sample collection and sample preparation: The marine sediment samples collected at sampling point A in Hangzhou Bay (Beilun District, Zhenhai District) were packed with clean aluminum foil and sealed in polyethylene bags, and then refrigerated in a portable refrigerator. Then transport the sample back to the laboratory, then place the sample in a freeze dryer to dry for 24 hours, take it out and pass it through a 100-mesh stainless steel sieve to obtain the sample to be tested, and place it in the desiccator for testing;

[0055] (2) Sampling and ultrasonic extraction: Weigh 2g of the sediment sample collected at sampling point A of Hangzhou Bay (Beilun District, Zhenhai District) processed in the above step (1), put it in a glass centrifuge tube, add 15mL volume Use n-hexane / ethyl acetate extractant wi...

Embodiment 2

[0089] Determination of 16 polyphthalates in sediment samples collected at sampling point B of Hangzhou Bay (Beilun District and Zhenhai District) in Ningbo:

[0090] (1) Sample collection and sample preparation: The sediment samples collected at sampling point B of Hangzhou Bay (Beilun District, Zhenhai District) in Ningbo were packed with clean aluminum foil and sealed in polyethylene bags, and then packed in a portable refrigerator. Transport back to the laboratory, then place the sample in a freeze dryer to dry for 12 hours, take it out and pass through an 80-mesh stainless steel sieve, and place it in a desiccator for testing; (2) Sampling and ultrasonic extraction: Weigh 2g of the above-mentioned step (1) and process it The sediment samples collected at sampling point B of Hangzhou Bay (Beilun District, Zhenhai District) in Ningbo were placed in a glass centrifuge tube, and 10 mL of n-hexane / ethyl acetate extractant with a volume ratio of 1:1 was added, and vortexed for 1...

Embodiment 3

[0098] Determination of 16 polyphthalates in sediment samples collected from Zhoushan Antarctic sea area:

[0099] (1) Sample collection and sample preparation: The sediment samples collected in the Zhoushan Antarctic sea area were packed with clean aluminum foil and sealed in polyethylene bags, and then transported back to the laboratory in a portable refrigerator, and then the samples were placed in the freezer. Dry it in a dryer for 18 hours, take it out and pass it through a 90-mesh stainless steel sieve, and place it in a dryer for testing;

[0100] (2) Sampling and ultrasonic extraction: Weigh 2g of the sediment sample collected from the Zhoushan Antarctic sea area treated in the above step (1), put it in a glass centrifuge tube, add 20mL of n-hexane / ethyl acetate with a volume ratio of 1:1 Ester extractant, vortex for 3min, ultrasonic extraction at 40°C with 350W power for 20min; when the background interference of sulfur-containing compounds in the sample, add 3g of co...

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Abstract

The invention relates to the technical field of marine sediment contamination detection, in particular to a dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of aphthalic acid ester environmental hormone in a marine sediment. The method comprises the following steps of: (1) sample collection, (2) sampling and ultrasonic extraction, (3) concentration, (4) dispersive solid-phase extraction purification, (5) concentration and constant volume, (6) detection by a gas chromatography-mass spectrometry detector, (7) standard curve drawing and (8) determination ofa recovery rate. The method is simple to operate; the ultrasonic extraction efficiency is high; pretreatment of a sample can be accomplished quickly; graphitized carbon black is used as a solid-phaseadsorbent for the first time; the dispersive solid-phase extraction efficiency is high; a purification effect is good; the method is higher in sensitivity, recovery rate and repeatability; a detection limit of 16 phthalic acid esters is 0.1-0.25 micrograms per kg; the recovery rate is 78-117%; a relative standard deviation (n=5) is 2.4-6.8%; and the method can be applied to the accurate determination of a phthalic acid ester content in the marine sediment.

Description

technical field [0001] The invention relates to the technical field of marine sediment pollution detection, in particular to a dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method for phthalate ester environmental hormones in marine sediments. Background technique [0002] As an important class of environmental hormones, phthalates are widely distributed in various media such as the atmosphere, water, soil, sediment, food, animals and plants, and even the human body. They have estrogen-like effects, interfere with the endocrine system, and cause Abnormal reproduction, development, and behavior. It is mainly used as a plasticizer in food, textiles, and children's toys. It can also be used as a raw material for the production of chemical products such as pesticides, cosmetics, and lubricants. It has been listed as "priority pollutants" by many countries in the world. list". Although phthalate pollution has attracted global attention, it can ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/12G01N30/08
CPCG01N30/02G01N30/06G01N30/08G01N30/12G01N30/72G01N2030/062G01N2030/126
Inventor 胡红美李铁军张露郭远明孙秀梅郝青应忠真
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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