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A kind of detection method of sufentanil citrate synthetic raw material and impurity

A detection method and citric acid technology, which are applied in measurement devices, material separation, and analysis of materials, etc., can solve problems such as poor separation of impurities and inability to control the content of impurities from the source.

Active Publication Date: 2016-06-29
YICHANG HUMANWELL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The standard uses liquid chromatography to determine related substances. The disadvantage is that the separation effect of impurities is not good, and it is only used for the detection of impurities in the finished product of sufentanil citrate API, and the content of impurities cannot be controlled from the source.

Method used

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  • A kind of detection method of sufentanil citrate synthetic raw material and impurity
  • A kind of detection method of sufentanil citrate synthetic raw material and impurity
  • A kind of detection method of sufentanil citrate synthetic raw material and impurity

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Effect test

Embodiment 1

[0048] Take 140801 batches of 2-thiophenethanol in an appropriate amount as the test sample, then directly inject the sample, and record the chromatogram. Compare the impurity retention time on the chromatogram with the impurity retention time of the reference substance to qualitatively impurity. Then the impurities were quantified by using the area normalization method according to the peak area of ​​each related substance. The invention can qualitatively and quantitatively carry out qualitative and quantitative analysis of 3-thiophenethanol impurities in the 2-thiophenethanol raw material, thereby controlling the quality of the sufentanil citrate synthetic raw material 2-thiophenethanol. The test results are attached figure 2 , and its detection data are shown in Table 2.

[0049] Table 2.140801 batches of 2-thiophenethanol for testing gas phase detection data

[0050]

[0051]

[0052] Take an appropriate amount of the intermediate 2-thiopheneethyl bromide after t...

Embodiment 2

[0056] Take 140802 batches of 2-thiophenethanol in an appropriate amount as the test sample, then directly inject the sample, and record the chromatogram. Compare the impurity retention time on the chromatogram with the impurity retention time of the reference substance to qualitatively impurity. Then the impurities were quantified by using the area normalization method according to the peak area of ​​each related substance. The invention can qualitatively and quantitatively carry out qualitative and quantitative analysis of 3-thiophenethanol impurities in the 2-thiophenethanol raw material, thereby controlling the quality of the sufentanil citrate synthetic raw material 2-thiophenethanol. The test results are attached Figure 4 , and its detection data are shown in Table 4.

[0057] Table 4.140802 batches of 2-thiophenethanol for testing gas phase detection data

[0058]

[0059] Take an appropriate amount of the intermediate 2-thiopheneethyl bromide after the brominati...

Embodiment 3

[0064] Take 140901 batches of 2-thiophenethanol in an appropriate amount as the test sample, then directly inject the sample, and record the chromatogram. Compare the impurity retention time on the chromatogram with the impurity retention time of the reference substance to qualitatively impurity. Then the impurities were quantified by using the area normalization method according to the peak area of ​​each related substance. The invention can qualitatively and quantitatively carry out qualitative and quantitative analysis of 3-thiophenethanol impurities in the 2-thiophenethanol raw material, thereby controlling the quality of the sufentanil citrate synthetic raw material 2-thiophenethanol. The test results are attached Image 6 , and its detection data are shown in Table 6.

[0065] Table 6.140901 batches of 2-thiophenethanol test product gas phase detection data

[0066]

[0067] Take an appropriate amount of intermediate 2-thiopheneethyl bromide after the bromination r...

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Abstract

The invention provides a method for detecting sufentanil citrate synthesis raw materials and impurities. By utilizing gas chromatography, the retention time is provided for determining the types of impurities, and the content of impurities is determined by utilizing an area normalization method. The method specifically comprises the following steps: respectively performing sample introduction on a mixed solution of standard solutions, and performing chromatographic analysis on the standard solution of each substance; performing sample introduction on a test sample, recording the chromatogram, contrasting the impurity retention time on the chromatogram with the retention time of a standard sample, determining the nature of the impurities, quantifying the impurities according to the peak area of each related substance by adopting the area normalization method, and performing qualitative and quantitative detection on the synthesis raw materials and impurities. The method is simple, and a good guarantee is provided for controlling the impurities in a finished sufentanil citrate product.

Description

technical field [0001] The invention relates to a drug impurity inspection method, in particular to a sufentanil citrate synthesis raw material and an intermediate impurity inspection method. Background technique: [0002] Sufentanil citrate is a derivative of fentanyl citrate, which is a powerful opioid analgesic. Sufentanil citrate is a strong μ-opioid receptor agonist, and its affinity for μ-receptor is about 7-10 times greater than that of fentanyl citrate. The analgesic strength of this product is 75-125 times that of morphine, and 5-10 times that of fentanyl citrate. This product is a highly lipophilic drug with rapid onset after intravenous injection, T1 / 2π, T1 / 2α, T1 / 2β are 0.73-1.2, 13.7-17 and 140-158min respectively. The plasma protein binding rate is 92%, mainly combined with α1-acid glycoprotein. The apparent volume of distribution Vd is 1.7L / kg, and the clearance rate CL is 12.7ml / min / kg. Most of it is metabolized in the liver to form N-desalkylated and O-de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 李振洲汪汶钟丽君付蓉田军郑炜
Owner YICHANG HUMANWELL PHARMA