A kind of detection method of phthalates

A phthalic acid and detection method technology, applied in the detection field, can solve the problems of large amount of organic solvents used, low measurement accuracy, long detection time, etc., and achieve the effect of accurate and reliable results, fast analysis speed and improved detection efficiency

Active Publication Date: 2018-08-17
CHONGQING ACAD OF METROLOGY & QUALITY INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is: the method for detecting phthalates in the prior art has low measurement accuracy, relatively long detection time, requires different temperature gradients or The elution gradient to ensure the complete separation of each target substance, the relatively high cost of detection, and the technical problems of using a large amount of organic solvents provide a phthalic acid that can achieve rapid and effective separation and detection of various phthalates. A detection method for ester substances, which has the characteristics of saving detection time and cost, improving detection efficiency, and being green and environmentally friendly

Method used

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  • A kind of detection method of phthalates

Examples

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Effect test

Embodiment 1

[0029] Example 1: Detection of phthalates by ultra-high performance convergence chromatography-diode array detector method

[0030] First, cut the same plastic sample as the control example into 1mm×1mm fragments, accurately weigh 0.5 g of the sample fragments, place them in a 25 mL stoppered colorimetric tube, add 10 mL of n-hexane accurately, ultrasonically extract for 30 min, and extract the solution through 0.45 After filtration by a μm organic membrane, the sample was injected into ultra-high performance convergence chromatography for analysis. The ultra-high performance convergence chromatography conditions: neutral, C18 SB packing with a particle size of 1.8 μm, the column length is 15 cm; the system back pressure is 12.41 MPa, and the chromatographic conditions are: The column temperature was 65°C, the injection volume was 3 μL, the mobile phase A was supercritical carbon dioxide, the mobile phase B was acetonitrile, and the column flow rate was 1.5 mL / min. Mobile phas...

Embodiment 2

[0032] Example 2: Detection of phthalates by ultra-high performance convergence chromatography-mass spectrometry

[0033] Cut the same plastic sample as the comparative example into fine particles with a single particle ≤ 0.02 g, accurately weigh 0.5 g of the sample particle, put it in a 25 mL stoppered colorimetric tube, add 10 mL of n-hexane accurately, ultrasonically extract for 60 min, and extract The liquid was filtered through a 0.45 μm organic membrane, and then injected into an ultra-high performance convergence chromatography for analysis. The chromatographic conditions: neutral, C18 SB packing with a particle size of 1.8 μm, the column length of the chromatographic column was 15 cm; the system back pressure was 13.10 MPa, and the chromatographic column The temperature was 55°C, the injection volume was 1 μL, the mobile phase A was supercritical carbon dioxide, the mobile phase B was acetonitrile, and the column flow rate was 1.0 mL / min. Mobile phase elution gradient ...

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Abstract

The invention discloses a detection method of phthalate matters. The detection method comprises the following steps: firstly carrying out elution by virtue of an ultra-high performance combined-phase chromatograph, wherein the elution conditions are as follows: the sample feeding quantity is 0.5-5 microliters, a stationary phase of a chromatographic column is a C18 filler, a mobile phase A is supercritical CO2, a mobile phase B is acetonitrile, the temperature of the chromatographic column in the detection process is maintained at 45-65 DEG C, and the column flow rate is 1.0mL / min-2.0mL / min; and detecting the eluted components by virtue of a diode array detector, a mass spectrometry detector or a tandem mass spectrometry detector, wherein the detection wavelength of a diode array is 220nm-250nm, and the detection mass numbers of the mass spectrometry detector and the tandem mass spectrometry detector are 40au-500au. By virtue of the detection method, the separation detection of multiple phthalates can be realize within 10 minutes, the detection efficiency is high, and the error rate of a result is less than 10%; and the use amount of an organic solvent is greatly reduced, so that the detection method is relatively environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a detection method of phthalates. Background technique [0002] Phthalate esters act like estrogen in humans and animals, and can interfere with endocrine. All countries in the world have restricted the scope and amount of their use. At present, the main detection methods of phthalate plasticizers include gas chromatography (CN104165945A), liquid chromatography (CN101788539A) and methods coupled with mass spectrometry (CN101858897A, CN102520091A, CN103630624A), ion mobility spectrometry (CN101852766A), Infrared spectroscopy (CN 101482505A), fluorescence method (CN105424663A), absorbance photometry (CN105203473A), etc. However, in the existing methods, the spectroscopic method cannot accurately characterize the target substance, the measurement accuracy is low, and the practical application is limited. The chromatographic method mainly faces the following problems ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 李武林李根容龙梅李小辉李沿飞陆嘉莉赵加雄邹孝马艳
Owner CHONGQING ACAD OF METROLOGY & QUALITY INST
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