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Purification preparation method of sulfopeptide indicator

An indicator and sample technology, which is applied in the field of purification and preparation of sulfopeptide indicators, can solve the problems of the influence of seawater pH value and total alkalinity on the accurate measurement, the cumbersome operation of the indicator purification method, and the limitation of the wide application of photometric method. Low cost, easy operation, good purification and preparation effect

Pending Publication Date: 2022-03-01
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently commercially available sulfopeptide indicators contain a certain amount of impurities, which have different effects on the measurement results (Yao, W.; Liu, X; Byrne, R.H. Impurities in indicators used for spectrophotometric seawater pH measurements: Assessment and remedies. Mar. Chem .2007, 107, 167-172), while the existing indicator purification methods are cumbersome to operate and have small yields, resulting in extremely high price and difficulty in obtaining the purified pH indicator (Liu, X.; Patsavas, M.C.; Byrne, R.H.Purification and characterization of meta-Cresol purple forspectrophotometric seawater pH measurements.Environ.Sci.Technol.2011,45,4862-4868.), thus limiting the wide application of photometry, the accurate determination of seawater pH and total alkalinity is greatly affected

Method used

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  • Purification preparation method of sulfopeptide indicator
  • Purification preparation method of sulfopeptide indicator
  • Purification preparation method of sulfopeptide indicator

Examples

Experimental program
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Effect test

Embodiment 1

[0025] The m-cresyl violet indicator is purified and prepared by using the present invention.

[0026] Weigh 98.07 mg of a certain brand of m-cresyl violet indicator into a sample bottle, add 4 mL of N,N-dimethylformamide, mix well, let stand for 5 minutes, ultrasonicate for 10 minutes, pass through a 0.22 μm filter membrane and place in in the syringe. Inject the sample in the syringe into the fast liquid phase preparative chromatograph for detection and separation. The organic phase in the mobile phase is acetonitrile, and the inorganic phase is ultrapure water. The gradient elution procedure is used. The procedure is shown in Table 1, and the flow rate is 40mL / min . The separation column used for analysis and detection is SΛNTΛITECHNOLOGIES SEPA Flash spherical C18 rapid separation column, the specifications are: column size 90g, particle size 40-60μm, pore size The detection wavelength is 434nm. Collect the purified samples separated by the rapid preparative liquid chr...

Embodiment 2

[0031] Purify and prepare the phenol red indicator by using the present invention.

[0032]Weigh 48.28mg of a certain brand of phenol red indicator into a sample bottle, add 1mL of N,N-dimethylformamide, mix well, let stand for 5min, sonicate for 10min, pass through a 0.22μm filter membrane and place in a centrifuge tube middle. Inject the sample in the syringe into the fast liquid phase preparative chromatograph for detection and separation. The organic phase in the mobile phase is acetonitrile and the inorganic phase is ultrapure water. The gradient elution program is used. The program is shown in Table 2, and the flow rate is 40mL / min . The separation column used for analysis and detection is SΛNTΛITECHNOLOGIES SEPA Flash spherical C18 rapid separation column. The model specifications are: column size 90g, particle size 40-60μm, pore size The detection wavelength is 400nm. Collect the purified samples separated by rapid preparative liquid chromatography at 33 to 36 minu...

Embodiment 3

[0037] This embodiment includes the following steps:

[0038] 1) Weigh 40 mg of thymol blue and place it in a sample bottle, add 1 to 10 mL of N,N-dimethylformamide, mix well, let stand for 5 minutes, and ultrasonicate for 5 minutes; the prepared concentration of thymol blue is 50 ~100mmol / L;

[0039] 2) Take the sample in step 1) and filter it through a 0.22 μm filter membrane and place it in a syringe;

[0040] 3) Inject the sample in the syringe of step 2) into a fast liquid phase preparative chromatograph for detection and separation; when detecting in the fast liquid phase preparative chromatograph, the organic phase in the mobile phase is acetonitrile, and the inorganic phase is ultrapure water, Gradient elution procedure is adopted, the proportion of organic phase is 5%-90%; the chromatographic column used for separation is C18 rapid separation column, the particle size is 40-60 μm, and the pore size is When performing fast liquid phase preparative chromatographic de...

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Abstract

The invention discloses a purification preparation method of a sulfopeptide indicator, and relates to purification preparation of reagents. A rapid liquid phase preparative chromatography system is adopted to detect and separate the sulfopeptide indicator and impurities in the sulfopeptide indicator, and a rotary evaporator and a nitrogen blowing concentrator are adopted to recover and prepare the purified sulfopeptide indicator. The method comprises the following steps: weighing a sulfopeptide indicator, dissolving the sulfopeptide indicator in N, N-dimethylformamide, carrying out ultrasonic treatment, filtering, and determining and separating in preparative liquid chromatography; and collecting the separated purified sample, transferring the purified sample to a rotary evaporator by using acetonitrile, carrying out rotary evaporation to a certain volume, transferring the sample to a nitrogen blowing instrument by using acetonitrile, carrying out nitrogen blowing to a certain volume, transferring the sample to a glass watch glass by using acetonitrile, sealing the glass watch glass by using aluminum-foil paper, reserving small ventilation holes in the aluminum-foil paper, and drying. Different elution procedures and detection wavelengths are selected according to different types of sulfopeptide indicators. The method is simple, convenient and rapid to operate, high in purification rate and high in yield, and can directly and effectively separate the sulfopeptide indicator from impurities to obtain the high-purity sulfopeptide indicator.

Description

technical field [0001] The invention relates to the purification and preparation of reagents, in particular to a method for the purification and preparation of a sulfopeptide indicator. Background technique [0002] Since the industrial revolution, the global average surface ocean acidity has increased by 26% (Byrne, R.H. Measuring Ocean Acidification: New Technology for a New Era of Ocean Chemistry. Environ. Sci. Technol. 2014, 48, 5352-5360), the average pH of surface seawater Annual decrease of 0.0019 (Intergovernmental Panel on Climate Change. Climate Change 2013: The Physical Science Basis. Working Group I Contribution to the Fifth Assessment Report of the IPCC. Final Draft.; IPCC: Geneva, Switzerland, 2013.). The absorption of carbon dioxide by seawater changes the chemical properties of the ocean, and the continuous increase in seawater acidity is called ocean acidification (Caldeira, K.; Wickett, M.E. Oceanography: Anthropogenic carbon and ocean pH. Nature 2003, 425(...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N30/06
CPCG01N1/28G01N30/06
Inventor 马剑李杭茜陈钊英刘宝敏
Owner XIAMEN UNIV