CN103868868A - Cisatracurium besilate content testing method - Google Patents
Cisatracurium besilate content testing method Download PDFInfo
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- CN103868868A CN103868868A CN201410115646.4A CN201410115646A CN103868868A CN 103868868 A CN103868868 A CN 103868868A CN 201410115646 A CN201410115646 A CN 201410115646A CN 103868868 A CN103868868 A CN 103868868A
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- atracurium
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- benzene sulphur
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Abstract
The invention discloses a cisatracurium besilate content testing method which comprises the following steps: respectively weighing a test substance and a reference substance in a measuring flask, adding hydrochloric acid for dissolving and metering a volume to a scale, shaking up to prepare a corresponding solution, finally, measuring the solution according to an ultraviolet-visible spectrophotometry, measuring absorbance at a place of a maximum adsorption wavelength of 280nm, and calculating the content of cisatracurium besilate according to an anhydrous substance. According to the cisatracurium besilate content testing method, the solution is simply and conveniently prepared, no organic solvent is used, and the pollution to the environment and the harm to a human body are small. The cisatracurium besilate content testing method is higher in testing speed, and the time of testing each batch of products in average only needs 30 min. A place of a maximum adsorption wavelength of 280 nm is selected, so that the testing accuracy is ensured. The cost of a reagent used in a process of checking each batch of samples does not exceed 20 yuan; the testing cost of each batch of samples by adopting a high-performance liquid chromatography method is not less than 200 yuan, so that the cost of enterprises is greatly lowered.
Description
Technical field
The invention belongs to pharmaceutical chemistry technical field, be specifically related to a kind of benzene sulphur along atracurium Content Test method.
Background technology
Now in the industry use benzene sulphur along atracurium Content Test method be: with octadecyl silane be filling agent; Taking 1.02% potassium dihydrogen phosphate buffer solution (with phosphorus acid for adjusting pH value to 3.1)-methyl alcohol-acetonitrile (75:5:20) as mobile phase A, taking 1.02% potassium dihydrogen phosphate buffer solution (with phosphorus acid for adjusting pH value to 3.1) ,-methyl alcohol-acetonitrile (50:30:20) is as Mobile phase B, and according to the form below carries out gradient elution; Detection wavelength is 280nm.
Get benzene sulphur along the about 10mg of atracurium, accurately weighed, be placed in 25ml volumetric flask, add mobile phase A and dissolve and quantitatively dilute and make the solution that approximately contains 0.4mg in every 1ml, precision measures 20ml, and injection liquid chromatography, records chromatogram; Separately get benzene sulphur along atracurium reference substance, be measured in the same method, calculate by dry product, containing C
53h
72n
2o
122C
6h
5o
3s should be 96.0%～102.0%.
This method of inspection mobile phase preparation time is long, and be 18 hours every batch of proving time, makes work efficiency low.And Expenses of laboratory examination is higher.
Summary of the invention
Goal of the invention: the present invention is directed to deficiency, propose a kind of detection time short, expend little and to environment and human body without the benzene sulphur of injury along atracurium Content Test method.
Technical scheme: a kind of benzene sulphur of the present invention, along atracurium Content Test method, comprises the steps:
(1) precision takes in test sample 9.5～10.5mg to 200ml measuring bottle, adds dissolving with hydrochloric acid and is settled to scale, shakes up, and makes in every 1ml approximately containing the need testing solution along atracurium 0.0475～0.0525mg;
(2) separately get benzene sulphur along in atracurium reference substance 9.5～10.5mg to 200ml measuring bottle, be settled to scale with dissolve with hydrochloric acid solution, shake up, make in every 1ml the approximately reference substance solution along atracurium 0.0475～0.0525mg containing benzene sulphur;
(3) get above-mentioned solution and measure according to " UV-VIS spectrophotometry ", measure absorbance log at its maximum absorption wavelength 280nm place, calculate benzene sulphur along atracurium content by dry product.
As preferably, described in described step (1) and (2), concentration of hydrochloric acid solution is 0.1mol/L.
Beneficial effect: this method solution preparation is easy, and use less than organic solvent, less for environmental pollution and human injury.It checks speed, and average every batch of examination and test of products only needs 30 minutes.Choose absorption maximum 280nm place, also ensured the accuracy of inspection.In every batch of checkout procedure, the expense of agents useful for same is no more than 20 yuan, and every batch of Expenses of laboratory examination of high-efficient liquid phase technique is not less than 200 yuan, and this also greatly reduces the cost of enterprise.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
A kind of benzene sulphur, along atracurium Content Test method, comprises the steps:
(1) precision takes in about 10mg to the 200ml measuring bottle of test sample, adds 0.1mol/L dissolving with hydrochloric acid and is settled to scale, shakes up, and makes in every 1ml approximately containing the need testing solution along atracurium 0.05mg;
(2) separately get benzene sulphur along in about 10mg to the 200ml measuring bottle of atracurium reference substance, be settled to scale with 0.1mol/L dissolve with hydrochloric acid solution, shake up, make in every 1ml the approximately reference substance solution along atracurium 0.05mg containing benzene sulphur;
(3) get above-mentioned solution and measure according to " UV-VIS spectrophotometry ", measure absorbance log at its maximum absorption wavelength 280nm place, calculate benzene sulphur along atracurium content by dry product.
Embodiment 2
A kind of benzene sulphur, along atracurium Content Test method, comprises the steps:
(1) precision takes in about 9.5mg to the 200ml measuring bottle of test sample, adds 0.1mol/L dissolving with hydrochloric acid and is settled to scale, shakes up, and makes in every 1ml approximately containing the need testing solution along atracurium 0.0475mg;
(2) separately get benzene sulphur along in about 9.5mg to the 200ml measuring bottle of atracurium reference substance, be settled to scale with 0.1mol/L dissolve with hydrochloric acid solution, shake up, make in every 1ml the approximately reference substance solution along atracurium 0.0475mg containing benzene sulphur;
(3) get above-mentioned solution and measure according to " UV-VIS spectrophotometry ", measure absorbance log at its maximum absorption wavelength 280nm place, calculate benzene sulphur along atracurium content by dry product.
Embodiment 3
A kind of benzene sulphur, along atracurium Content Test method, comprises the steps:
(1) precision takes in about 10.5mg to the 200ml measuring bottle of test sample, adds 0.1mol/L dissolving with hydrochloric acid and is settled to scale, shakes up, and makes in every 1ml approximately containing the need testing solution along atracurium 0.0525mg;
(2) separately get benzene sulphur along in about 10.5mg to the 200ml measuring bottle of atracurium reference substance, be settled to scale with 0.1mol/L dissolve with hydrochloric acid solution, shake up, make in every 1ml the approximately reference substance solution along atracurium 0.0525mg containing benzene sulphur;
(3) get above-mentioned solution and measure according to " UV-VIS spectrophotometry ", measure absorbance log at its maximum absorption wavelength 280nm place, calculate benzene sulphur along atracurium content by dry product.
In order to verify the feasibility of the above-mentioned method of inspection, now adopt spectrophotometry inspection technique to carry out methodological study to inspection, with feasible, the reliable and validity of prove method, effectively ensure drug quality.
1.1 checking contents
Inspection specimen in use, reference substance source and lot number:
Benzene sulphur is along atracurium lot number:
20130501source:
raw material workshop
Benzene sulphur is along atracurium reference substance lot number:
20120909content:
99.2%source:
our factory
1.1.1 testing conditions
(DY322035-00) measure according to " spectrophotometry inspection technique standard practice instructions ", measure its absorbance log at its maximum absorption wavelength 280nm place, calculate content by external standard method with absorbance log.
1.1.2 linear relationship
Precision takes benzene sulphur along in atracurium reference substance 25mg to 25ml measuring bottle, and each precision measures 1ml and puts respectively in 50ml, 25ml, 20ml, 10ml, 5ml measuring bottle, uses hydrochloric acid solution (0.1mol/L) dissolved dilution to scale, to shake up; Measure the regression equation (n=6) of absorption value A and concentration C (mg/ml).(seeing attached list 1)
Subordinate list 1
?linear relationship
1.1.3 repeated
Precision measures benzene sulphur along in atracurium 10mg to 200ml measuring bottle, adds the dilution of 0.1mol/L hydrochloric acid solution and is settled to scale, shakes up, and makes need testing solution.Measure according to 4.4.1 condition, calculate repeatability (RSD≤2%).(seeing attached list 2)
Subordinate list 2 replica test results
1.1.4 the recovery
Precision takes benzene sulphur along each three parts of atracurium reference substance 8,10,12mg, is placed in respectively 200ml measuring bottle, to scale, measures (RSD≤2%, the recovery >=98.5%) according to 4.4.1 condition with 0.1mol/L hydrochloric acid solution (0.1mol/L) dissolved dilution.(seeing attached list 3)
Subordinate list 3 recovery (W theoretical amount/W amount of recording * 100%)
Checking conclusion: this verification method indices meets examination requirements, shows that the method is feasible, selects the method to carry out benzene sulphur along atracurium assay result accurately and reliably.
Claims (2)
1. benzene sulphur, along an atracurium Content Test method, is characterized in that: comprise the steps:
(1) precision takes in test sample 9.5～10.5mg to 200ml measuring bottle, adds dissolving with hydrochloric acid and is settled to scale, shakes up, and makes in every 1ml approximately containing the need testing solution along atracurium 0.0475～0.0525mg;
(2) separately get benzene sulphur along in atracurium reference substance 9.5～10.5mg to 200ml measuring bottle, be settled to scale with dissolve with hydrochloric acid solution, shake up, make in every 1ml the approximately reference substance solution along atracurium 0.0475～0.0525mg containing benzene sulphur;
(3) get above-mentioned solution and measure according to " UV-VIS spectrophotometry ", measure absorbance log at its maximum absorption wavelength 280nm place, calculate benzene sulphur along atracurium content by dry product.
2. a kind of benzene sulphur according to claim 1, along atracurium Content Test method, is characterized in that: described in step (1) and (2), concentration of hydrochloric acid solution is 0.1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410115646.4A CN103868868A (en) | 2014-03-26 | 2014-03-26 | Cisatracurium besilate content testing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410115646.4A CN103868868A (en) | 2014-03-26 | 2014-03-26 | Cisatracurium besilate content testing method |
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| CN103868868A true CN103868868A (en) | 2014-06-18 |
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| CN201410115646.4A Pending CN103868868A (en) | 2014-03-26 | 2014-03-26 | Cisatracurium besilate content testing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105277647A (en) * | 2015-12-03 | 2016-01-27 | 上药东英（江苏）药业有限公司 | Method for determining content of cisatracurium besylate of raw materials by HPLC (High Performance Liquid Chromatography) |
| CN110220861A (en) * | 2019-06-04 | 2019-09-10 | 上海信谊万象药业股份有限公司 | A kind of measuring method of Azasetron hydrochloride drug content |
-
2014
- 2014-03-26 CN CN201410115646.4A patent/CN103868868A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 国家药典委员会: "《中华人民共和国药典 2010年版》", 30 August 2012 * |
| 韦艳丽等: "HPLC 法测定原料苯磺酸顺阿曲库铵的有关物质与含量", 《长春理工大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105277647A (en) * | 2015-12-03 | 2016-01-27 | 上药东英（江苏）药业有限公司 | Method for determining content of cisatracurium besylate of raw materials by HPLC (High Performance Liquid Chromatography) |
| CN110220861A (en) * | 2019-06-04 | 2019-09-10 | 上海信谊万象药业股份有限公司 | A kind of measuring method of Azasetron hydrochloride drug content |
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Application publication date: 20140618 |