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Method for measuring content of vitamin D2 in vitamin D2 injection by UPCC (Ultra Performance Convergence Chromatography)

A technology for vitamins and injections, applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of poor reproducibility, large error in results, waste of manpower, material resources and time, etc., to save detection cost and time, and achieve high accuracy , specificity and good linear effect

Active Publication Date: 2019-12-31
苏州市药品检验检测研究中心
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method for the determination of vitamin D2 content in vitamin D2 injection is now the first method for the determination of vitamin D in the 2015 edition of the Chinese Pharmacopoeia Four General Rules 0722. This method uses normal phase chromatography, system suitability test, preparation of reference substances, and mixed reference substances The preparation process of the method is very cumbersome, all of which need to be processed by water bath heating and nitrogen passage, and the calculation process is complicated, the result error is large, the reproducibility is poor, and the mobile phase uses a large amount of organic solvents to pollute the environment, wasting a lot of manpower, material resources and time.

Method used

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  • Method for measuring content of vitamin D2 in vitamin D2 injection by UPCC (Ultra Performance Convergence Chromatography)
  • Method for measuring content of vitamin D2 in vitamin D2 injection by UPCC (Ultra Performance Convergence Chromatography)
  • Method for measuring content of vitamin D2 in vitamin D2 injection by UPCC (Ultra Performance Convergence Chromatography)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The content of vitamin D2 in vitamin D2 injection was determined by this example, and its specificity was verified.

[0029] 1. The detection conditions are as follows:

[0030] Column: ACQUITY UPC 2TM BEH, 1.7μm, 3.0×100mm;

[0031] Mobile phase: supercritical CO 2 And tetrahydrofuran (95:5);

[0032] Back pressure: 2700psi;

[0033] Detection wavelength: 254nm;

[0034] Flow rate: 1.0ml / min;

[0035] Column temperature: 45°C;

[0036] Injection volume: 5 μl.

[0037] 2. Each solution is prepared as follows:

[0038] (1) Standard stock solution: Accurately weigh 12.5mg of vitamin D2 reference substance, put it in a 50ml brown measuring bottle, immediately dissolve it with n-hexane and dilute to the mark, the concentration of this solution is about 0.25mg / ml. Accurately weigh 12.5mg of vitamin D3 reference substance and place it in a 50ml brown measuring bottle, dissolve it with n-hexane immediately and dilute to the mark, shake well, the concentration of this ...

Embodiment 2

[0046] Using the detection conditions, reference substance solution and determination method in Example 1, the linear relationship investigation was carried out.

[0047] Accurately measure vitamin D2 standard stock solutions, add n-hexane to dilute to prepare reference solutions containing vitamin D2 12.5, 20, 25, 37.5, 50, and 100 μg / ml respectively, and measure according to the chromatographic conditions under the content determination item. Area (A) carries out regression analysis to concentration (C), as table 1, image 3 shown.

[0048] Table 1 Vitamin D2 linear relationship results

[0049]

[0050] It can be seen that the concentration of vitamin D2 has a good linear relationship in the range of 13.019-104.148 μg / ml, and the correlation coefficient R 2 = 0.9999.

Embodiment 3

[0052] Adopt the detection condition, reference substance solution and assay method among the embodiment one, examine accuracy and precision on the basis of embodiment one, embodiment two.

[0053] 1. Inspection of accuracy

[0054]Sample recovery rate test: Accurately measure 9 parts of the test solution with known content of each component, and each group of 3 parts is divided into three groups, and each group is added with 0.8ml, 1.0ml of vitamin D2 standard stock solution according to the three concentrations of low, medium and high respectively. ml, 1.2ml, add n-hexane to dilute to the mark, shake well, accurately measure 5μl and inject into the convergence chromatograph, record the chromatogram, calculate the recovery rate and RSD of vitamin D2, the average recovery rate of vitamin D2 is 98.76% , RSD is 1.86%, indicating that the accuracy of the present invention is high.

[0055] 2. Inspection of precision

[0056] Precisely measure 5 μl of vitamin D2 reference substa...

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Abstract

The invention discloses a chromatographic method for rapidly measuring the content of vitamin D2 in a vitamin D2 injection. The effect that the content of vitamin D2 in a complex component sample is measured rapidly and accurately is finally achieved through skillful optimization for a chromatographic condition by using an ultra performance convergence chromatography. The chromatographic method comprises the following steps of (1) preparing a system suitability solution; (2) preparing a reference solution; and (3) preparing a test solution. The content of vitamin D2 in the vitamin D2 injectionis calculated by using a standard curve of vitamin D2. According to the chromatographic method for rapidly measuring the content of vitamin D2 in the vitamin D2 injection disclosed by the invention,the vitamin D2 can be rapidly separated within 15 min and the content of vitamin D2 can be accurately measured; and the method has the advantages of good specificity and linear relation, high accuracydegree, fast detection speed, high sensitivity, good reproducibility and environmental protection.

Description

technical field [0001] The invention relates to a method for measuring vitamin D2 content in vitamin D2 injection by using ultra-high performance convergence chromatography (UPCC), using supercritical CO 2 As the mobile phase and clever optimization of chromatographic conditions, the content of vitamin D2 in vitamin D2 injection can be determined quickly and accurately. Background technique [0002] Vitamin D2 injection is clinically used for the prevention and treatment of vitamin D deficiency, chronic hypocalcemia, hypophosphatemia, rickets and osteomalacia with chronic renal insufficiency, familial hypophosphatemia and parathyroid Treatment of hypogonadism and for the treatment of acute, chronic and potentially postoperative tetany and idiopathic tetany. [0003] The method for the determination of vitamin D2 content in vitamin D2 injection is now the first method for the determination of vitamin D in the 2015 edition of the Chinese Pharmacopoeia Four General Rules 0722....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34G01N2030/047Y02P20/54
Inventor 郝刚马冬阳顾炳仁陈卫邹松邢以文周坚王亚琼陈蓉张斌顾晓红苏静华朱乃军
Owner 苏州市药品检验检测研究中心
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