阅读说明：本技术 一种盐酸贝尼地平片含量均匀度的测定方法 (Method for measuring content uniformity of benidipine hydrochloride tablets ) 是由 王熙红 林丽丽 杨淑萍 陈莉 于 2019-10-14 设计创作，主要内容包括：本发明涉及一种盐酸贝尼地平片含量均匀度的测定方法,解决了现有盐酸贝尼地平片含量均匀度的测定方法区分力差、操作复杂、检测时间长、对人员健康影响大的技术问题。本发明提供一种盐酸贝尼地平片含量均匀度的测定方法,包括以下步骤：取盐酸贝尼地平片1片,置100ml量瓶中,加甲醇-稀磷酸混合溶液适量,超声使盐酸贝尼地平溶解并稀释至刻度,摇匀,滤过,取续滤液作为供试品溶液。本发明广泛应用于盐酸贝尼地平片含量均匀度的检测。(The invention relates to a method for measuring content uniformity of a benidipine hydrochloride tablet, and solves the technical problems of poor discrimination, complex operation, long detection time and great influence on human health of the conventional method for measuring the content uniformity of the benidipine hydrochloride tablet. The invention provides a method for measuring content uniformity of benidipine hydrochloride tablets, which comprises the following steps: taking 1 tablet of benidipine hydrochloride, placing in a 100ml measuring flask, adding a proper amount of methanol-diluted phosphoric acid mixed solution, ultrasonically dissolving and diluting benidipine hydrochloride to scale, shaking up, filtering, and taking the subsequent filtrate as a test solution. The method is widely applied to the detection of the content uniformity of the benidipine hydrochloride tablets.)

1. A method for measuring content uniformity of benidipine hydrochloride tablets is characterized by comprising the following steps: taking 1 tablet of benidipine hydrochloride, placing in a 100ml measuring flask, adding a proper amount of methanol-diluted phosphoric acid mixed solution, ultrasonically dissolving and diluting benidipine hydrochloride to scale, shaking up, filtering, and taking the subsequent filtrate as a test solution.

2. The method for determining the content uniformity of the benidipine hydrochloride tablets as claimed in claim 1, wherein the concentration of the dilute phosphoric acid is 0.2%, and the volume ratio of the methanol to the dilute phosphoric acid is 1: 1.

3. The method for measuring the content uniformity of the benidipine hydrochloride tablets according to claim 1, wherein the method further comprises the following steps: and (3) measuring the test solution by using a high performance liquid chromatography, wherein the chromatographic conditions and the system applicability test are as follows: chromatographic column using octadecylsilane chemically bonded silica as filler; using 0.05mol/L potassium dihydrogen phosphate solution (pH is adjusted to 3.0 by phosphoric acid) -methanol-tetrahydrofuran as mobile phase; detecting wavelength at 237nm, column temperature at 25 deg.C, adjusting flow rate to make peak retention time of benidipine hydrochloride about 20min, precisely measuring 10 μ l of filtrate, injecting into liquid chromatograph, and recording chromatogram;

taking another appropriate amount of benidipine hydrochloride reference substance, precisely weighing, dissolving with the above mixed solution, quantitatively diluting to obtain solution containing 0.08mg per 1ml, and determining by the same method;

calculating according to the peak area by an external standard method to obtain the product.

4. The method for measuring the content uniformity of the benidipine hydrochloride tablets as claimed in claim 3, wherein the chromatographic column is an Agilent Pursuit, 4.6 x 100mm, 3 μm or equivalent performance chromatographic column.

5. The method for measuring content uniformity of the benidipine hydrochloride tablet as claimed in claim 3, wherein the volume ratio of 0.05mol/L potassium dihydrogen phosphate solution (adjusted to pH 3.0 with phosphoric acid) in the mobile phase to methanol-tetrahydrofuran is 65:27: 8.

Technical Field

The invention relates to the technical field of pharmacy, in particular to a method for measuring content uniformity of benidipine hydrochloride tablets.

Background

Benidipine hydrochloride belongs to dihydropyridine calcium ion antagonists, and expands blood vessels by binding to dihydropyridine receptors that block cell membrane potential-dependent calcium ion channels, and preventing calcium ion influx into cells. Benidipine hydrochloride is widely used as a therapeutic drug for hypertension, renal essential hypertension, angina pectoris, and the like because it is safe and effective.

The content uniformity is a key parameter for evaluating the quality of the medicine and is also a key factor for examining the quality of the medicine according to the Chinese pharmacopoeia. The content is guaranteed for the whole batch of products, and the content uniformity is the difference between the content of each piece. However, the detection method has the following problems:

1. the existing method for measuring the content uniformity of the benidipine hydrochloride tablets in China is an ultraviolet method, and substances such as auxiliary materials and the like which have absorption at the wavelength influence the detection result, so that the interference factors are more, and the result accuracy is poor.

2. In the past, the content uniformity is detected by taking 1 sample, adding a solvent, grinding, and then quantitatively transferring to a volumetric flask to prepare a test solution. The traditional method has a complex operation process, the volatilization of organic solvents such as methanol and the like has great harm to the health of operators, and in addition, incomplete transfer also easily causes detection errors and inaccurate results.

3. The content uniformity detection method of the benidipine hydrochloride tablets in the Japanese pharmacopoeia is that 1 tablet of a sample is shaken until the benidipine hydrochloride is dissolved. The benidipine hydrochloride tablet is a coated tablet, so that the active ingredients of the coating layer can be dissolved by shaking for a long time, the detection time is long, and the benidipine hydrochloride tablet is not suitable for daily operation.

4. The benidipine hydrochloride has two crystal forms of alpha and beta, and has alpha type with pharmacological action. The chromatographic peak of the beta isomer is adjacent to the active ingredient, and improper selection of chromatographic conditions can cause the isomer to be combined with the main ingredient, thus causing high results.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, and provides a method for measuring the content uniformity of benidipine hydrochloride tablets, which is simple to operate, reliable in method, high in repeatability and high in accuracy and is verified by methodology according to the characteristics of the benidipine hydrochloride tablets.

The technical scheme adopted by the invention for solving the technical problem is as follows:

a method for measuring content uniformity of benidipine hydrochloride tablets comprises the following steps: taking 1 tablet of benidipine hydrochloride, placing in a 100ml measuring flask, adding a proper amount of methanol-diluted phosphoric acid mixed solution, ultrasonically dissolving and diluting benidipine hydrochloride to scale, shaking up, filtering, and taking the subsequent filtrate as a test solution.

Preferably, the concentration of the dilute phosphoric acid is 0.2%, and the volume ratio of the methanol to the dilute phosphoric acid is 1: 1.

Preferably, the steps further comprise: and (3) measuring the test solution by using a high performance liquid chromatography, wherein the chromatographic conditions and the system applicability test are as follows: chromatographic column using octadecylsilane chemically bonded silica as filler; using 0.05mol/L potassium dihydrogen phosphate solution (pH is adjusted to 3.0 by phosphoric acid) -methanol-tetrahydrofuran as mobile phase; detecting wavelength at 237nm, column temperature at 25 deg.C, adjusting flow rate to make peak retention time of benidipine hydrochloride about 20min, precisely measuring 10 μ l of filtrate, injecting into liquid chromatograph, and recording chromatogram;

taking another appropriate amount of benidipine hydrochloride reference substance, precisely weighing, dissolving with the above mixed solution, quantitatively diluting to obtain solution containing 0.08mg per 1ml, and determining by the same method;

calculating according to the peak area by an external standard method to obtain the product.

Preferably, the column is an Agilent Pursuit, 4.6X 100mm, 3 μm or equivalent performance column.

Preferably, the mobile phase is a 0.05mol/L solution of potassium dihydrogen phosphate (pH adjusted to 3.0 with phosphoric acid) -methanol-tetrahydrofuran volume ratio of 65:27: 8.

The invention has the beneficial effects that:

compared with the prior art, the method for measuring the content uniformity of the benidipine hydrochloride tablets is simple to operate, reliable, small in influence on human health, high in repeatability and high in accuracy through methodology verification.

Detailed Description

The present invention will be further described with reference to specific examples to assist understanding of the invention. The method used in the invention is a conventional production method if no special provisions are made; the starting materials used, unless otherwise specified, are conventional commercial products.

Examples

A method for measuring content uniformity of benidipine hydrochloride tablets comprises the following steps:

taking 1 tablet of benidipine hydrochloride, placing in a 100ml measuring flask, adding a proper amount of methanol-diluted phosphoric acid mixed solution, ultrasonically dissolving and diluting benidipine hydrochloride to scale, shaking up, filtering, and taking the subsequent filtrate as a test solution.

The concentration of the dilute phosphoric acid is 0.2 percent, and the volume ratio of the methanol to the dilute phosphoric acid is 1: 1.

And (3) measuring the test solution by using a high performance liquid chromatography, wherein the chromatographic conditions and the system applicability test are as follows: a column packed with octadecylsilane bonded silica gel (Agilent Pursuit, 4.6X 100mm, 3 μm or equivalent performance column); using 0.05mol/L potassium dihydrogen phosphate solution (pH is adjusted to 3.0 by phosphoric acid) -methanol-tetrahydrofuran (65: 27: 8) as a mobile phase; detecting wavelength at 237nm, column temperature at 25 deg.C, adjusting flow rate to make peak retention time of benidipine hydrochloride about 20min, precisely measuring 10 μ l of filtrate, injecting into liquid chromatograph, and recording chromatogram;

taking another appropriate amount of benidipine hydrochloride reference substance, precisely weighing, dissolving with the above mixed solution, quantitatively diluting to obtain solution containing 0.08mg per 1ml, and determining by the same method;

the content of each tablet is obtained by calculating the peak area according to an external standard method, the content average value of the content uniformity of the benidipine hydrochloride tablet is 98.9 percent of the marked amount, the RSD value is 0.89 percent, the content average value meets the specification, the establishment of the method is verified through methodology, and the method is high in repeatability and accuracy.

In conclusion, compared with the prior art, the method for measuring the content uniformity of the benidipine hydrochloride tablets is simple to operate and reliable, and has high repeatability and high accuracy through methodology verification.

However, the above description is only an embodiment of the present invention, and the scope of the present invention should not be limited by this, and all equivalent changes and modifications made in the claims of the present invention should be covered by the present invention.