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Determination method of amount of phthalic acid esters

A technology for the determination of phthalic acid and its determination method, which is applied in the field of determination of the total amount of phthalates, can solve problems such as difficult detection of phthalates and complex metabolite components, and achieve sensitivity High, simple operation, good stability

Active Publication Date: 2012-04-18
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are methods such as gas phase, liquid phase, gas-mass spectrometry, and liquid-mass spectrometry to detect phthalates. It is widely used, but these methods are all for the detection of one or several phthalates, but because phthalates are a class of substances, including a large number of types, some products are clearly stipulated at home and abroad It cannot be contained, and even if it is used, the types are different. It is difficult to detect phthalates one by one, and the metabolites are complex. Therefore, a method can be established to detect the total amount of phthalates. The amount can not only effectively evaluate whether food, especially oily food, is contaminated by phthalate plasticizers, but also provide technical support for the internal exposure evaluation of phthalates in humans. At present, there is no relevant research at home and abroad. research reports, therefore, establishing a method to determine the total amount of phthalates will fill the gap in this field

Method used

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  • Determination method of amount of phthalic acid esters
  • Determination method of amount of phthalic acid esters
  • Determination method of amount of phthalic acid esters

Examples

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Effect test

Embodiment 1

[0038] The determination of the total amount of phthalic acid substances in the oil sample of embodiment 1

[0039] (1) Use phthalic acid standard stock solution to prepare standard solutions with phthalic acid concentrations of 0.05, 0.1, 1, 10, 25, 50, and 100 mg / L. Draw 10 μ L of the standard solution of each concentration and inject it into high-performance liquid chromatography for analysis, and obtain the peak area of ​​the high-performance liquid chromatography obtained from the corresponding concentration, and obtain the standard curve of the peak area-mass concentration of the phthalic acid standard substance and the linear regression equation Y=63331X+ 47465, R 2 =0.9995, and the lowest detection limit was obtained as 0.02mg / L.

[0040] (2) After mixing the sample evenly, weigh 2.0g, put it in a reflux bottle, add 10ml of methanol and mix evenly, then add 10mL of KOH solution with a concentration of 2mol / L, heat it in a water bath at 85°C for 2.5h, and finally remov...

Embodiment 2

[0058] The determination of the total amount of phthalic acid substances in the urine of embodiment 2

[0059] (1) Use phthalic acid standard stock solution to prepare standard solutions with phthalic acid concentrations of 0.05, 0.1, 1, 10, 25, 50, and 100 mg / L. Draw 10 μ L of the standard solution of each concentration and inject it into a high-performance liquid chromatograph for analysis, and obtain the phthalic acid standard substance peak area-mass concentration standard curve and linear regression equation Y=63331X+47465, R 2 =0.9995, and the lowest detection limit was obtained as 0.02mg / L.

[0060] (2) Take the urine sample and centrifuge it at 12000rpm / min for 20min to take the supernatant, take 1ml, add 15μL of β-glucuronide hydrolase, and shake at a constant temperature of 37°C for 12h.

[0061] (3) The enzymolysis solution was inactivated in boiling water at 100°C. After cooling, centrifuge at 12000rpm / min for 20min to take the supernatant, put it in a reflux bott...

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Abstract

The invention discloses a determination method of an amount of phthalic acid esters. The determination method comprises the following steps: carrying out alkaline hydrolysis on samples in order; acidifying to converse all phthalic acid esters in samples into phthalic acid; extracting by ethyl acetate; drying out and redissolving with methanol; filtering by organic filter membrane to obtain sampleliquids; determining phthalic acid content in the sample liquids by high performance liquid chromatography; carrying out conversion according to a phthalic acid standard substance peak area- mass concentration standard curve and a linear regression equation to calculate out the amount of phthalic acid esters in the samples. The determination method of the amount of phthalic acid esters has advantages of simple pre-treatment, rapidness and high sensitivity, is beneficial for large-scale sample determination and suitable for determination of the amount of phthalic acid ester in oil food, like edible oil, seasoning sauce for instant noodle and convenient rice noodle, and urine biological specimen.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography analysis, and in particular relates to a method for measuring the total amount of phthalates. Background technique [0002] Phthalic acid esters (Phthalic Acid Esters, referred to as PAEs, alias phthalates) are an important class of organic compounds. Because they can increase the plasticity and strength of plastics, they are widely used in toys, food packaging materials, and medical blood bags. and hoses, vinyl flooring and wallpaper, cleaners, lubricants, personal care products such as nail polish, hair sprays, soaps and shampoos, and hundreds of other products. [0003] In plastics, PAEs and polyolefin plastic molecules are connected by hydrogen bonds or van der Waals forces, and they retain their relatively independent chemical properties, and gradually migrate from plastics to food with changes in time, temperature and other conditions, resulting in food contamination. Contamin...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 柳春红孙远明张明明杨金易王弘杨艺超徐小艳
Owner SOUTH CHINA AGRI UNIV
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