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Method for separating and detecting m-cresol and p-cresol content through ultrahigh liquid chromatography and application thereof

An ultra-high liquid chromatography, p-cresol technology, applied in the field of p-cresol content, ultra-high liquid chromatography separation and detection of m-cresol, can solve the problem of β-cyclodextrin blocking pipelines and columns, easy to crystallize , low solubility of β-cyclodextrin, etc., to achieve the effect of reducing analysis cost, easy operation and reducing solvent consumption

Active Publication Date: 2021-03-19
RACHEM CHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese literature "Ultra-high performance liquid chromatography β-cyclodextrin mobile phase additive method to analyze 7 kinds of phenolic compounds in mainstream cigarette smoke" and Chinese invention patent CN200810301862.2 adding β-cyclodextrin to the mobile phase Separation of phenol and p-cresol, but β-cyclodextrin has low solubility in water and is easy to crystallize, which can easily lead to the precipitation of β-cyclodextrin to block the pipeline and column

Method used

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  • Method for separating and detecting m-cresol and p-cresol content through ultrahigh liquid chromatography and application thereof
  • Method for separating and detecting m-cresol and p-cresol content through ultrahigh liquid chromatography and application thereof
  • Method for separating and detecting m-cresol and p-cresol content through ultrahigh liquid chromatography and application thereof

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Experimental program
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Effect test

Embodiment 1

[0044] Ultra-high liquid chromatography experiment: Waters H-Class ultra-high liquid chromatography, PDA diode array detector;

[0045] Chromatographic column: XBridge BEH phenylhexyl column (100×2.1mm, 1.7μm);

[0046] Mobile phase: The volume ratio of organic phase to aqueous phase is 40:60, gradient elution; the organic phase is methanol, and the aqueous phase is chromatographic grade phosphoric acid water;

[0047] Flow rate: 0.2mL / min;

[0048] Detection wavelength: 270nm;

[0049] Column temperature: 40°C;

[0050] Injection volume: 1μL;

[0051] (1) Test procedure for detection: Weigh 20 mg m-cresol and p-cresol standard samples respectively, dissolve them in methanol in a 10 mL volumetric flask, dilute to volume, shake well, and use a 0.2 μm filter membrane as the standard solution for later use.

[0052] (2) Weigh 25 mg of phenolic resin or waste water from the synthesis process, dissolve it in methanol in a 10 mL volumetric flask, constant volume, shake well, and...

Embodiment 2

[0056] Ultra-high liquid chromatography experiments:

[0057] Waters H-Class ultra-high liquid chromatography, PDA diode array detector;

[0058] Chromatographic column: XBridge BEH phenylhexyl column (100×2.1mm, 1.7μm);

[0059] Mobile phase: The volume ratio of organic phase to aqueous phase is 40:60, gradient elution; the organic phase is methanol, and the aqueous phase is chromatographic grade phosphoric acid water;

[0060] Flow rate: 0.3mL / min;

[0061] Detection wavelength: 270nm;

[0062] Column temperature: 40°C;

[0063] Injection volume: 1μL;

[0064] Test steps for detection:

[0065] (1) Weigh 20 mg m-cresol and p-cresol standard samples respectively, dissolve them in methanol in a 10 mL volumetric flask, dilute to volume, shake well, and use a 0.2 μm filter membrane as standard solutions for later use.

[0066] (2) get standard solution, inject ultra-high liquid chromatograph, analyze according to above-mentioned chromatographic condition, record collection...

Embodiment 3

[0068] Ultra-high liquid chromatography experiments:

[0069] Waters H-Class ultra-high liquid chromatography, PDA diode array detector;

[0070] Chromatographic column: XBridge BEH phenylhexyl column (100×2.1mm, 1.7μm);

[0071] Mobile phase: The volume ratio of organic phase to aqueous phase is 40:60, gradient elution; the organic phase is methanol, and the aqueous phase is chromatographic grade phosphoric acid water;

[0072] Flow rate: 0.2mL / min;

[0073] Detection wavelength: 270nm;

[0074] Column temperature: 40°C;

[0075] Injection volume: 3μL;

[0076] Test steps for detection:

[0077] (1) Weigh 20 mg m-cresol and p-cresol standard samples respectively, dissolve them in methanol in a 10 mL volumetric flask, dilute to volume, shake well, and use a 0.2 μm filter membrane as standard solutions for later use.

[0078] (2) get standard solution, inject ultra-high liquid chromatograph, analyze according to above-mentioned chromatographic condition, record collection...

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Abstract

The invention discloses a method for separating and detecting m-cresol and p-cresol content by adopting a phenyl column through ultra-high performance liquid chromatography. The method comprises the following steps of: adopting a chromatographic column taking triple bond bonding as a stationary phase, taking an organic phase-aqueous phase buffer solution as a mobile phase, and ensuring that the flow rate is 0.1-0.3 mL / min, wherein the detection wavelength is 210-400 nm; the column temperature is 10-40 DEG C; the sample size is 0.5-5 mu L; respectively carrying out ultrahigh liquid chromatography on standard samples with different concentration gradients and samples to be detected, establishing a linear regression curve, and substituting the peak area measured by the samples to be detectedinto the regression curve to obtain the contents of the cresol and the p-cresol in the samples to be detected. According to the method, the analysis time is greatly shortened, the operation is simpleand convenient, pre-column derivatization is not needed, and the purpose of product quality control can be quickly and accurately achieved. In addition, the solvent consumption is reduced, and the analysis cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical detection and analysis, and relates to a method for separating and detecting the content of m-cresol and p-cresol by ultra-high liquid chromatography. Background technique [0002] Cresol is usually composed of o-cresol, m-cresol and p-cresol, and is an important fine chemical intermediate. Among them, m-cresol and p-cresol are usually separated and detected by gas chromatography and polar chromatographic column HP-INNOWAX due to their similar boiling points. But when the water content of the sample is large, the test sample will cause great harm to the chromatographic column. Since the structures and physical and chemical properties of m-cresol and p-cresol are very similar, the most widely used C18 column for reverse chromatography has no obvious separation effect in the separation of m-cresol and p-cresol. Currently, they are combined method to calculate total content, while the BEH Phenyl c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/64G01N30/74
CPCG01N30/02G01N30/06G01N30/64G01N30/74
Inventor 黄玲董栋张宁
Owner RACHEM CHINA CO LTD
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