A dispersive solid-phase extraction-gas chromatography-mass spectrometry detection method for phthalate ester environmental hormones in seafood

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 method for detecting phthalate environmental hormones in seafood by dispersed solid phase extraction-gas chromatography-mass spectrometry. Background technique [0002] Phthalates, also called phthalates, are an important type of organic matter formed by the esterification of phthalic anhydride and various alcohols, mainly including natural sources and artificial synthesis, and are widely used as plasticizers in plastics. The amount accounts for about 80% of the total amount of plasticizer. Since the phthalate and the plastic matrix are connected by hydrogen bonds and van der Waals forces, they are easily released into the atmosphere, water, soil and other environments, and ultimately endanger human health through the enrichment of the food chain. Studies have shown that phthalate compounds have estrogen-like activity, which can produce clear reproduction, devel...

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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%)

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