High performance liquid chromatographic detection method for 3-cyanopyridine and 4-methylpyridine in 4-cyanopyridine

A high-performance liquid chromatography and cyanopyridine technology, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problem of difficulty in querying high-performance liquid chromatography detection methods, difficult to control the content of 4-cyanopyridine, inability to solvent peaks and other problems. Impurity peak separation and other problems, to achieve the effect of short analysis time, accurate and reliable detection results, and fast dissolution speed

Active Publication Date: 2016-10-26
江苏悦兴医药技术有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to completely separate the peak time of 4-cyanopyridine from the solvent peak and impurity peak, improve the peak shape, and then accurately control the content of 4-cyanopyridine. At present, it is difficult to find 4-cyanopyridine Correlative HPLC detection method for 3-cyanopyridine and 4-picoline in pyridine
[0005] The feature of the present invention is to overcome the high polarity of 4-cyanopyridine, which leads to early peaks in high performance liquid chromatography, which cannot be well separated from solvent peaks and impurity peaks, and the peak shape is not good, so it is difficult to control Difficulties with 4-cyanopyridine content

Method used

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  • High performance liquid chromatographic detection method for 3-cyanopyridine and 4-methylpyridine in 4-cyanopyridine
  • High performance liquid chromatographic detection method for 3-cyanopyridine and 4-methylpyridine in 4-cyanopyridine
  • High performance liquid chromatographic detection method for 3-cyanopyridine and 4-methylpyridine in 4-cyanopyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] A kind of 3-cyanopyridine, 4-picoline high performance liquid chromatography detection method in 4-cyanopyridine:

[0067] (1) Preparation of system suitability solution: Accurately weigh 50 mg each of 3-cyanopyridine and 4-picoline, place in a 50ml measuring bottle, dissolve and dilute to the mark with acetonitrile, shake well, and make 3-cyanopyridine with a concentration of 1mg / ml, 4-picoline concentration of 1mg / ml homogeneous solution: as impurity stock solution; then accurately weigh 50mg of 4-cyanopyridine and put it in a 50ml measuring bottle, then add impurity stock solution 0.5ml, use acetonitrile Dissolve and dilute to the mark, shake well, and make a homogeneous solution with 4-cyanopyridine concentration of 1 mg / ml, 3-cyanopyridine concentration of 10 μg / ml, and 4-picoline concentration of 10 μg / ml, which is suitable for the system sexual solution;

[0068] (2) Preparation of the test solution: Accurately weigh 50 mg of 4-cyanopyridine and put it in a 50ml...

Embodiment 2

[0085] Except changing the flow rate in the detection condition to be 0.8ml / min, other steps and conditions are all the same as in Example 1.

[0086] According to the above test conditions, accurately measure 10 μl of the system suitability solution and inject it into the liquid chromatograph, record the chromatogram, see figure 2 And table 2; Precision measures need testing solution and contrast solution each 10 μ l injects liquid chromatograph, record chromatogram, calculate 3-cyanopyridine, 4-picoline content in need testing product with peak area by self contrast method . The content of 3-cyanopyridine was 0.055%, 4-picoline was not detected.

[0087] The separation effect of 3-cyanopyridine, 4-cyanopyridine and 4-picoline under the condition of table 2, embodiment 2

[0088] Chromatographic peak

[0089] The results show that the resolution of 3-cyanopyridine, 4-cyanopyridine and 4-picoline in the detection method of the present invention is 2.65 and 9.00, a...

Embodiment 3

[0091] Except changing the flow rate to 1.2ml / min in the detection conditions, other steps and conditions are the same as in Example 1.

[0092] According to the above detection conditions, accurately measure 10 μl of the system suitability solution and inject it into the liquid chromatograph, record the chromatogram, see image 3 And table 3; Precision measures need testing solution and contrast solution each 10 μ l injects liquid chromatograph, record chromatogram, calculate 3-cyanopyridine, 4-picoline content in need testing product with peak area by self contrast method . The content of 3-cyanopyridine was 0.055%, 4-picoline was not detected.

[0093] The separation effect of 3-cyanopyridine, 4-cyanopyridine and 4-picoline under table 3, embodiment 3 conditions

[0094] Chromatographic peak

[0095] The results show that the resolution of 3-cyanopyridine, 4-cyanopyridine and 4-picoline in the detection method of the present invention is 2.38, 11.80, and the num...

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Abstract

The invention discloses a high performance liquid chromatographic detection method for 3-cyanopyridine and 4-methylpyridine in 4-cyanopyridine. The high performance liquid chromatographic detection method comprises the following steps: (1) preparing a system applicable solution; (2) preparing a test solution; 3) preparing a contrast solution. The system applicable solution, the test solution and the contrast solution are detected respectively by adopting high performance liquid chromatography. The detection condition is as follows: octadecylsilane chemically bonded silica is used as a filling agent of a chromatographic column; a mobile phase A is modified buffer salt, and is prepared by adding 20 mmol of potassium dihydrogen phosphate and 2.4 ml of triethylamine into 1000 ml of water and adjusting the pH value to 6.0-8.0 with phosphoric acid; a mobile phase B is an organic phase, and adopts gradient elution; the flow rate is 0.5-1.5 ml / min; the column temperature is 10-40 DEG C; the detection wave length is 200-300 nm; the injected sample volume is 10 [mu]l. The separation degree of 3-cyanopyridine, 4-cyanopyridine and 4-methylpyridine in the detection method are all 2.0 or above, the theoretical plate number is high, the symmetry is good, and the condition that the accuracy of the detection results is influenced by interference between the components is effectively avoided; meanwhile, the detection method has the advantages of being accurate and reliable in detection result, short in analysis time, simple and convenient to operate, and the like.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a high-performance liquid chromatography detection method, a high-performance liquid chromatography detection method of 3-cyanopyridine and 4-picoline in 4-cyanopyridine. Background technique [0002] 4-cyanopyridine is the starting material for the synthesis of topirastat. The molecular formula of 4-cyanopyridine C 6 h 4 N 2 , the molecular weight is 104.11, and its structural formula is as follows: [0003] [0004] The purpose of the present invention is to completely separate the peak time of 4-cyanopyridine from the solvent peak and impurity peak, improve the peak shape, and then accurately control the content of 4-cyanopyridine. At present, it is difficult to find 4-cyanopyridine Correlative HPLC detection method of 3-cyanopyridine and 4-picoline in pyridine. [0005] The feature of the present invention is to overcome the high polarity of 4-cyanopyridine, which le...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 林海荣翟富民陆学山陈建丽包华兰
Owner 江苏悦兴医药技术有限公司
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