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High performance liquid detection method of D-potassium erythorbate

A technology of potassium ascorbate and high performance liquid phase, which is applied in the field of high performance liquid phase detection of potassium D-erythorbate, can solve the problems of inability to accurately detect the content of potassium D-erythorbate and content interference of titration method, and achieve the detection time Short, good peak shape, high sensitivity results

Active Publication Date: 2020-06-26
新拓洋生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing disclosed technology, there is no relevant detection method for potassium D-erythorbate. In GB1886.28, the detection method of analogue sodium D-erythorbate, there is an iodine titration method; Zhang Zhigang invented a kind of content of sodium D-erythorbate The detection method uses a chromatographic column filled with octadecylsilane-bonded silica gel, uses potassium dihydrogen phosphate solution-methanol as the mobile phase, and detects with an ultraviolet detector; currently, as a new chemical substance, D-potassium erythorbate has no According to any relevant literature on the determination of modern analytical instruments, iodine titration cannot accurately detect the content of D-potassium erythorbate during the detection process, and the titration test content is easily interfered by other substances that react with iodine. Accurate quantitative detection method of potassium D-erythorbate to meet the needs of the quality control process

Method used

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  • High performance liquid detection method of D-potassium erythorbate
  • High performance liquid detection method of D-potassium erythorbate
  • High performance liquid detection method of D-potassium erythorbate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Carry out HPLC analysis under the following chromatographic conditions, measure the content of D-potassium erythorbate:

[0026] Chromatographic column: HILIC Amide 250mm×4.6mm, 5um, polyacrylamide bonded silica gel column;

[0027] Mobile phase: 20mmol / L potassium dihydrogen phosphate buffer solution and acetonitrile mixed solution=25:75; pH value is 6.5-6.7;

[0028] Diluent: a mixed solution of acetonitrile and water with a volume ratio of 75:25;

[0029] Flow rate: 1.0mL / min;

[0030] Column temperature: 40°C;

[0031] Detector: UV detector;

[0032] Detection wavelength: 240nm;

[0033] Injection volume: 10uL.

[0034] 2. Preparation of mobile phase:

[0035] Weigh 2.72g of potassium dihydrogen phosphate, dissolve and dilute to 1000ml with ultra-pure water, add 3L of chromatographically pure acetonitrile, mix well, filter with 0.45um organic filter membrane, degas it by ultrasonic, and store it in a brown bottle.

[0036] 3. Preparation of diluent:

[00...

Embodiment 2

[0045] In order to verify the feasibility and accuracy of the above-mentioned example one, a linear experiment was carried out, and the experimental concentration took 5mg / L, 10mg / L, 50mg / L, 100mg / L, 150mg / L and 200mg / L of D-potassium erythorbate standard solution , using exactly the same chromatographic conditions as in Example 1, the measurement results are shown in Table 1.

[0046] Table 1 Linearity experiment results

[0047]

[0048] Table 1 Standard curve regression equation y=9938.7022x+5546.7719, R2=0.9997; good linearity.

[0049] From figure 1 It can be seen that the retention time of 7.148min is the peak of D-potassium erythorbate, and the rest are miscellaneous peaks. The peak time of the main peak is appropriate, the number of theoretical plates is greater than 5000, and the separation from miscellaneous peaks is good.

[0050] From figure 2 It can be seen that the retention time of 7.147min is the peak of D-potassium erythorbate, and the rest are miscella...

Embodiment 3

[0052] In order to verify the feasibility and accuracy of the above-mentioned embodiment 1, a precision test is carried out. The test adopts a concentration of D-potassium erythorbate standard solution prepared at 100ug / mL, and continuous sample injection is performed for 6 times. Conditions, the measurement results are shown in Table 2.

[0053] Table 2 Precision test results

[0054]

[0055] It can be seen from Table 2 that the RSD of the peak area is less than 2%, so the stability of the instrument is good.

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Abstract

The invention provides a high performance liquid chromatography detection method of D-potassium erythorbate, and the detection chromatographic conditions are as follows: high performance liquid chromatography is used for analysis, and a polyacrylamide bonded silica gel chromatographic column is adopted; a mixed solution of a phosphate buffer solution and acetonitrile is taken as a mobile phase; amixed solution of acetonitrile and water is used as a diluent, and an ultraviolet detector is used for detection. The sample pretreatment steps are simple, the D-potassium erythorbate does not need tobe derived, the detection time is short, and the method provided by the invention has high sensitivity; according to the method provided by the invention, the content of the D-potassium erythorbate can be well measured, and the requirement on quality control in the production process can be met.

Description

technical field [0001] The invention relates to the field of chromatographic detection, in particular to a high-efficiency liquid phase detection method for potassium D-erythorbate. Background technique [0002] D-potassium erythorbate, scientific name: D-2,3,5,6-tetrahydroxy-2-ethylene acid-γ-lactone potassium salt, also known as potassium erythorbate, potassium erythorbate. The molecular formula is: C 6 h 7 KO 6 . The product is white powder or granules, odorless, slightly salty, soluble in water. Potassium D-erythorbate is a new type of antioxidant, which can effectively maintain the color and natural flavor of food, prolong the shelf life, and also inhibit the formation of carcinogenic nitrosamines in food. The product can also be used in wool spinning, electroplating, cigarettes, feed processing, industrial water treatment and petrochemical industries. In the existing disclosed technology, there is no detection method related to potassium D-erythorbate. In GB1886....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/34G01N30/06G01N30/74
CPCG01N30/88G01N30/34G01N30/06G01N30/74G01N2030/884
Inventor 秦天苍郭金权张建国史立军吴娜石明卫徐琳杜志豪陈倩倩孙秋月王峥魏艳芳王星陈婧桀王向蒙
Owner 新拓洋生物工程有限公司
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