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

A technology of phthalates and phthalic acid, which is applied in the field of seafood pollution detection, can solve the problems of unsuitable for batch sample processing, poor detection sensitivity, large adsorption dose, etc., and achieve satisfactory recovery rate and reproducibility , high sensitivity, simple operation

Active Publication Date: 2018-05-08
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Purification by gel permeation chromatography requires the use of a large amount of elution solvent and a large investment in equipment; although the detection cost of the chromatographic column is low, the amount of adsorbent used each time is large, and it needs to be filled manually, and the reproducibility is low. Poor; the current commercialized solid phase extraction cartridges have been widely used in sample purification, but the process of activation, sample loading, rinsing, and elution of the extraction column is still required, which takes a long time and is not suitable for batch samples In addition, in recent years, dispersive solid-phase extraction purification has been widely used in the field of food testing, but for phthalates in aquatic products, the current method reported in the literature is to use N-propylethylenediamine adsorbent Dispersed in 2mL of isopropanol or acetonitrile, but the research found that when the color of the aquatic product extract is dark, using N-propylethylenediamine as the adsorbent, the color of the extract basically does not change, and the expected impurity removal effect cannot be achieved. And the detection sensitivity is very poor. For example, among the commercially available fish, shrimp, and oysters detected by Wang Wenwen et al., five kinds of dimethyl phthalate, diethyl phthalate, and diphthalate with higher detection rates Isobutyl, dibutyl phthalate, and di-2-ethylhexyl phthalate were not detected
According to further experiments, when N-propylethylenediamine is dispersed in isopropanol, in addition to diisobutyl phthalate, diethoxyethyl phthalate, and di-2-phthalate The recovery rate of ethylhexyl ester was slightly higher (70-78%), and the recovery rate of other 13 kinds of phthalates was very low (23-64%); when N-propylethylenediamine was dispersed in acetonitrile, 16 The recoveries of all phthalates were very low (26-43%)

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Determination of 16 polyphthalates in perch samples collected in Dongtou sea area of ​​Wenzhou:

[0060](1) Sample collection and sample preparation: Pack the perch samples collected in the Dongtou sea area of ​​Wenzhou with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, and then put the samples back into the laboratory. Remove the scales and skin, take the muscle along the back, cut it into block samples with a volume no larger than 0.5cm×0.5cm×0.5cm, homogenize it with a high-speed tissue grinder, and obtain the sample to be tested, and store it in a freezer at -18°C. to be tested;

[0061] (2) Sampling and ultrasonic extraction: Weigh 2g of the perch sample collected in the Wenzhou Dongtou sea area treated in the above step (1), put it in a glass centrifuge tube, add 15mL of n-hexane / dichloride with a volume ratio of 1:1 Methane extractant, vortex for 2min, ultrasonic extraction at 35°C ...

Embodiment 2

[0094] Determination of 16 kinds of polyphthalates in samples of imitation Penaeus harbachii purchased from an aquatic product wharf in Zhoushan:

[0095] (1) Sample collection and sample preparation: The imitation prawn samples purchased from a certain aquatic product wharf in Zhoushan 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 removed. Remove the head, shell, and appendages, take the muscle, cut it into block samples with a volume not greater than 0.5cm×0.5cm×0.5cm, homogenize it with a high-speed tissue grinder, obtain the sample to be tested, and store it in a freezer at -18°C , to be tested;

[0096] (2) Sampling and ultrasonic extraction: Weigh 2g of the imitative Penaeus prawn sample purchased from an aquatic product wharf in Zhoushan that has been processed in the above step (1), put it in a glass centrifuge tube, add 10mL of n-hexane / Dichlorom...

Embodiment 3

[0104] Determination of 16 polyphthalates in swimming crab samples purchased from a farmer's market in Zhoushan:

[0105] (1) Sample collection and sample preparation: Pack the swimming crab samples purchased from a farmer’s market in Zhoushan with clean aluminum foil and seal them in a polyethylene bag, then transport them back to the laboratory in a portable refrigerator, and then remove the heads and remove the samples. The shell and appendages were removed, and the muscle was taken, cut into block samples with a volume not larger than 0.5cm×0.5cm×0.5cm, homogenized with a high-speed tissue grinder, and the samples to be tested were obtained, and stored at -18°C for testing ;

[0106] (2) Sampling and ultrasonic extraction: Weigh 2 g of Portunus crab samples purchased from a farmer’s market in Zhoushan that have been processed in the above step (1), place them in a glass centrifuge tube, and add 20 mL of n-hexane / dichloromethane with a volume ratio of 1:1 Extraction agent,...

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Abstract

The invention relates to the technical field of seafood contamination detection, in particular to a dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method of a phthalic acid ester environmental hormone in seafood. The method comprises the following steps of: (1) sample collection, (2) sampling and ultrasonic extraction, (3) concentration, (4) dispersive solid-phaseextraction purification, (5) concentration and constant volume, (6) detection by a gas chromatography-mass spectrometry detector, (7) standard curve drawing and (8) determination of a 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-phase adsorbent for thefirst 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 0.15-0.3 micrograms per kg; the recovery rate is 74-116%; a relative standard deviation (n=5) is 2.5-6.9%; and the method can be applied to the accurate determination of a phthalicacid ester content in the seafood.

Description

technical field [0001] The invention relates to the technical field of seafood pollution detection, in particular to a dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method for phthalate ester environmental hormones in seafood. Background technique [0002] Phthalate, also known as phthalate, is an important organic compound formed by the esterification of phthalic anhydride and various alcohols. It mainly includes natural sources and artificial synthesis, and is widely used in plasticizers. The dosage accounts for about 80% of the total plasticizer usage. Since phthalates are connected to the plastic matrix by hydrogen bonds and van der Waals forces, they are easily released into the atmosphere, water, soil and other environments, and eventually enriched through the food chain to endanger human health. Studies have shown that phthalates have estrogen-like activity, which can produce clear reproduction, developmental toxicity and teratogeni...

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 胡红美张露李铁军郭远明孙秀梅郝青金衍健
Owner MARINE FISHERIES RES INST OF ZHEJIANG