Method for ion chromatography detection of acarbose

An acarbose and ion chromatography technology, applied in measurement devices, material separation, instruments, etc., can solve the problems of large solvent or impurity interference, quantitative defects, long peak time, etc., and achieve short analysis time and good selectivity. , the effect of high sensitivity

Inactive Publication Date: 2017-06-20
JIANGNAN UNIV
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Problems solved by technology

Since acarbose only absorbs at the end of the UV spectrum, it can only be measured with a low wavelength below 210nm when using a UV detector, which has the disadvantages of large interference from solvents or impurities, and long peak elapse time.
However, the differential refractive index detector has the disadvantages of low sensitivity, high temperature-affected baseline stability, and inability to perform gradient elution.
When using an evaporative light scattering detector, there are limitations in quantification due to its nonlinearity

Method used

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  • Method for ion chromatography detection of acarbose
  • Method for ion chromatography detection of acarbose
  • Method for ion chromatography detection of acarbose

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Experimental program
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Effect test

Embodiment 1

[0025] The instrument used in the experiment is ISC 5000 ion chromatograph from Thermo Fisher Company, and the chromatographic conditions are: chromatographic column: Thermo CarboPac PA20 anion exchange column, including analytical column (250mm × 4mm id) and guard column (50mm × 4mm id); column temperature: 30°C; injection volume: 20 μL. Isocratic elution was carried out with 300mmol / L sodium hydroxide solution as the eluent, the flow rate was 0.5mL / min, the pulsed amperometric detector adopted the sugar standard four-potential waveform, and the ion chromatogram of acarbose was shown in figure 1 .

[0026] Dilute the mixed standard solution mother liquor to different multiples, and perform detection and analysis under the chromatographic conditions of this embodiment. Take the concentration of acarbose as the abscissa and the peak area as the ordinate to draw a standard working curve, and by regression calculation, obtain the standard curve as Y=1.1264X+0.0021, the correlati...

Embodiment 2

[0028] The instrument used in the experiment is ISC 5000 ion chromatograph from Thermo Fisher Company, and the chromatographic conditions are: chromatographic column: Thermo CarboPac PA10 anion exchange column, including analytical column (250mm × 4mm id) and guard column (50mm × 4mm id); column temperature: 35°C; injection volume: 20 μL. Isocratic elution was carried out with 200mmol / L sodium hydroxide solution as the eluent, the flow rate was 1.0mL / min, the pulsed amperometric detector adopted the sugar standard four-potential waveform, and the ion chromatogram of acarbose was shown in figure 2 .

Embodiment 3

[0030] The instrument used in the experiment is ISC 5000 ion chromatograph from Thermo Fisher Company, and the chromatographic conditions are: chromatographic column: Thermo CarboPac PA20 anion exchange column, including analytical column (250mm × 4mm id) and guard column (50mm × 4mm id); column temperature: 30°C; injection volume: 20 μL. Isocratic elution was carried out with 200mmol / L sodium hydroxide solution as the eluent, the flow rate was 0.5mL / min, the pulsed amperometric detector adopted the sugar standard four-potential waveform, and the ion chromatogram of acarbose was shown in image 3 .

[0031] In addition, the inventors respectively investigated the separation and elution effects of 50, 100, 200, 300 and 500 mmol / L NaOH eluents on acarbose. When the NaOH concentration was 50 and 100mmol / L, the peak of acarbose was late and the peak shape was flat; when the NaOH concentration was increased to 500mmol / L, the peak of acarbose was earlier, which was different from t...

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Abstract

The invention discloses a method for ion chromatography detection of acarbose and belongs to the field of analysis and detection. The method utilizes high efficiency anion exchange chromatogram column separation and pulsed amperometric detector-based detection, utilizes a sodium hydroxide solution as a mobile phase and utilizes an external standard method for quantitative analysis. The lowest detection limit of acarbose is 0.15 microgram / L, a recovery rate is 96.8% to 102.2%, and reproducibility is in a range of 0.59% to 0.84% (RSD, n=5). The method has the advantages of high detection sensitivity and fast analysis speed and can be used for content detection and quality evaluation of acacosose products in related industries.

Description

technical field [0001] The invention relates to a method for detecting acarbose by ion chromatography, belonging to the field of analysis and detection. Background technique [0002] Acarbose (Acarbose) is a biosynthetic pseudotetrasaccharide (structural formula such as figure 1 ), is an α-glucosidase inhibitor developed in recent years. It can inhibit the activity of α-glucosidase in the brush border of small intestinal wall cells, thereby inhibiting the hydrolysis of polysaccharides and oligosaccharides, delaying and reducing the production of glucose, and controlling the rise of blood sugar concentration after meals. As a drug for the clinical treatment of type Ⅱ diabetes, acarbose has the characteristics of novel mechanism of action, good clinical curative effect, and low toxicity and side effects, and has a broad market prospect. [0003] At present, high performance liquid chromatography (HPLC) is mainly used for the detection of acarbose, and the detectors used incl...

Claims

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Application Information

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IPC IPC(8): G01N30/96
CPCG01N30/96
Inventor 朱松戴军陈尚卫
Owner JIANGNAN UNIV
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