Method for quantitative analysis of sucrose-6-acetate through combination of mid-infrared spectrum and vector angle

A technology of infrared spectroscopy and vector angle, applied in the field of quantitative analysis of compound infrared spectroscopy, to achieve the effect of not relying on spectral characteristic response, low detection limit, and good linear relationship

Active Publication Date: 2018-02-16
JK SUCRALOSE
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Problems solved by technology

[0003] The infrared light in the infrared transmission spectrum region can penetrate up to 30mm in the sample. Compared with the diffuse reflectance technique (Diffuse Reflectance Technique), the obtained spectral information is more abundant, but because Christiansen (Christiansen, 1884) cannot avoid The effect exists, and it is also severely restricted by information superposition. There are still few reports on quantitative application of infrared transmission spectroscopy using traditional KBr tablet and coating methods.

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  • Method for quantitative analysis of sucrose-6-acetate through combination of mid-infrared spectrum and vector angle
  • Method for quantitative analysis of sucrose-6-acetate through combination of mid-infrared spectrum and vector angle
  • Method for quantitative analysis of sucrose-6-acetate through combination of mid-infrared spectrum and vector angle

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preparation example Construction

[0047] Preparation of mixed solution

[0048] Mix solution 1 and solution 2 according to different volumes to prepare a series of mixed sample solutions of sucrose-sucrose-6-acetate in N,N-dimethylformamide (DMF) and record them as E1~E10;

[0049] Taking the synthetic liquids under different reaction times during the synthetic process of sucrose-6-acetate to obtain synthetic liquid samples;

[0050] Preparation of samples for mid-infrared spectroscopy

[0051] Step 2. Infrared Spectrum Collection of Samples

[0052] Select the infrared transmission mode and set the test parameters: the spectrum acquisition range is 450-4000cm -1, with a resolution of 4cm -1 , the data interval is 1cm -1 Under this condition, collect the DMF solution of above sucrose-6-acetate synthetic liquid, sucrose-6-acetate, the DMF solution of sucrose, DMF, the infrared spectrum of mixed solution sample respectively;

[0053] Step 3. Data processing method

[0054] (1) Import the spectral data of t...

experiment example

[0065] Experimental Instruments and Reagents

[0066] Micro-injector (5uL, long in Shanghai Laser Instrument), pipette gun (10-100uL, 100-1000uL), Frontier Fourier transform infrared spectrometer (Perkin Elmer, USA), Agilent 1200 high-performance liquid chromatography (Agilent Corporation, USA) ), far-infrared fast drying oven (WS70-1 type), electronic analytical balance (CP214 type).

[0067] Sucrose (AR), DMF (AR), tert-butylamine (AR), sucrose-6-acetate reference substance (purity 95.2%, determined by HPLC), potassium bromide (AR)

[0068] Preparation of sucrose-sucrose-6-acetate-DMF mixed solution

[0069] Preparation of reference solution

[0070] (1) Preparation of sucrose reference substance solution

[0071] Weigh 2.0112 g of the sucrose reference substance (AR, 99.5%) with an electronic analytical balance, add it into a small beaker, add an appropriate amount of DMF, and sonicate at 70° C. until the sucrose dissolves. After cooling to room temperature, it was tran...

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Abstract

A method for quantitative analysis of sucrose-6-acetate through combination of a mid-infrared spectrum and a vector angle includes a step 1, preparing a series of samples; step 2, collecting the infrared spectrums of the samples, which includes selecting an infrared transmission mode, setting test parameters, including setting the spectrum collection range to be 450-4000 cm<-1>, the resolution tobe 4 cm<-1>, and the data interval to be 1 cm<-1>, and under the condition, collecting mid-infrared spectrums of the series of samples, including a DMF solution of sucrose-6-acetate, a DMF solution ofsucrose, DMF and a mixed solution of sucrose-6-acetate; and step 3, treating data. The method can fast accurately measure the content of sucrose-6-acetate in a synthetic process. The method doesn't require sample pretreatment and big data modeling, is simple, and has the characteristics of independence to spectral signature response, low detection limit and wide application range.

Description

technical field [0001] The invention relates to the field of infrared spectrum quantitative analysis of compounds, in particular to a method for quantitative analysis of sucrose-6-acetate by combining mid-infrared spectrum with vector angle. Background technique [0002] Infrared spectroscopy, the most commonly used method for molecular characterization, is generally considered to have limited quantitative capabilities. Since the infrared spectrum is generated by the vibrational absorption of molecules in the infrared region, it has disadvantages such as weak energy, poor interpretation of the spectrum, and high detection limit, making direct quantitative analysis difficult. In recent years, with the popularization of attenuated total reflection (ATR) sampling, it is gradually used for quantification. Mid-infrared ATR quantification and secondary quantification based on multivariate statistics show that infrared spectroscopy has quantitative capabilities. [0003] The infr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/38G01N21/3577
CPCG01N1/38G01N21/3577
Inventor 姚志湘粟晖文毅潘浩然黄晓程杨晨
Owner JK SUCRALOSE
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