阅读说明：本技术 一种二甲硅油乳剂的含量测定方法 (Content determination method of dimeticone emulsion ) 是由 刘春燕 万华英 王祖焕 于 2021-07-28 设计创作，主要内容包括：本发明提供一种二甲硅油乳剂的含量测定方法,它包括如下步骤精密称定,置带塞(或旋盖)锥形瓶中,加盐酸溶液,精密加入正庚烷,振摇,将混合物分液分取正庚烷层,加无水硫酸钠振摇,滤过,澄清滤液作为供试品溶液。称取二甲基聚硅氧烷对照品,与供试品溶液同样操作,作为对照品溶液；取正庚烷,加无水硫酸钠振摇,滤过的澄清溶液作为空白溶液。照红外分光光度法测定,选择测定波长为1260cm～(-1)±2cm～(-1),0.5mm吸收池测得供试品溶液及对照品溶液的吸收度,计算含量。该方法含量测定结果准确,重复性和回收率良好,且该方法通过验证,可用二甲硅油乳剂样品的常规分析和质量控制。(The invention provides a content determination method of dimeticone emulsion, which comprises the following steps of precisely weighing, placing in a conical flask with a plug (or a screw cap), adding hydrochloric acid solution, precisely adding n-heptane, shaking, separating the mixture liquid and taking an n-heptane layer, adding anhydrous sodium sulfate, shaking, filtering, and clarifying the filtrate to be used as a test solution. Weighing a dimethyl polysiloxane reference substance, and taking the dimethyl polysiloxane reference substance as a reference substance solution in the same operation as the test substance solution; n-heptane was taken, anhydrous sodium sulfate was added and shaken, and the filtered clear solution was used as a blank solution. Measuring by infrared spectrophotometry, selecting measurement wavelength of 1260cm ‑1 ±2cm ‑1 And measuring the absorbances of the test solution and the reference solution by a 0.5mm absorption cell, and calculating the content. The method has accurate content measurement result, good repeatability and recovery rate, and can be used for routine analysis and quality control of the dimeticone emulsion sample through verification.)

1. A content determination method of a dimeticone emulsion is characterized by comprising the following steps: the method adopts n-heptane as a solvent, and adopts an infrared spectrophotometry to carry out determination, and comprises the following steps:

1) preparation of a test solution: taking the product which is about 50mg equivalent to the simethicone, and precisely weighing;

2) placing the mixture into a conical flask with a plug or a screw cap, adding 50ml of 1mol/L hydrochloric acid solution, precisely adding 25ml of n-heptane, shaking for 5 minutes by using force, transferring the mixture to a 125ml separating funnel, standing for 30 minutes, separating an n-heptane layer after layering, adding 3g of anhydrous sodium sulfate, shaking, filtering, and clarifying the filtrate to obtain a sample solution;

2) preparation of control solutions: precisely weighing about 50mg of dimethyl polysiloxane reference substance, and preparing by the same operation as the step 2) and the test solution;

3) preparation of a blank solution: 10ml of n-heptane is taken, 3g of anhydrous sodium sulfate is added for shaking, and the filtered clear solution is used as a blank solution;

4) the determination method comprises the following steps: selecting 1260cm wavelength by infrared spectrophotometry^-1±2cm^-1And measuring the absorbances of the test solution and the reference solution by a 0.5mm absorption cell, and calculating the content.

2. The method for measuring the content of a simethicone emulsion according to claim 1, wherein: the 0.5mm absorption pool is an HF-8 fixed liquid pool.

Technical Field

The invention relates to a content determination method of a dimeticone emulsion, which adopts an infrared spectrophotometry to determine the content of dimeticone in the dimeticone emulsion.

Background

As a common disease diagnosis method, gastric endoscopy and X-ray examination are increasingly applied, and along with the continuous development of medical science, the application of the method is increasingly wide, and in order to improve the definition of examination, thereby improving the accuracy of diagnosis and reducing the missed diagnosis and misdiagnosis rate, the application of an antifoaming agent for eliminating gastrointestinal tract gas and vesicular mucus in preoperative preparation is also increasingly applied. The simethicone is the most common medical antifoaming agent in medical circles at home and abroad, can obviously improve abdominal symptoms caused by gas in gastrointestinal tracts, quickly eliminate the gas in the gastrointestinal tracts and vesicular mucus, and improve the definition of gastric endoscopy and X-ray examination.

The dimeticone emulsion is used as an auxiliary medicine for gastroscopy and radioscopy; the simethicone has small surface tension, can change the surface tension of bubbles to break the bubbles, thereby eliminating the foams in the gastrointestinal tract and discharging the gas stored by the foams, thereby relieving flatulence. Eliminating bubble mucus in stomach, and improving definition of gastroscopy and radiology.

The method for measuring the content of the dimeticone emulsion in the existing national standard comprises the following steps: taking a proper amount (about 50mg of simethicone) of the product, precisely weighing, placing the product in a conical flask with a plug (or a screw cap), adding 50ml of 1mol/L hydrochloric acid solution, precisely adding 25ml of carbon tetrachloride, shaking for 5 minutes by force, transferring the mixture to a 125ml separating funnel, standing for 30 minutes, after layering, separating a carbon tetrachloride layer, adding 3g of anhydrous sodium sulfate, shaking, filtering, and clarifying filtrate to obtain a test solution. Carbon tetrachloride is used as a solvent, is a colorless toxic liquid, can dissolve various substances such as fat, paint and the like, is a volatile liquid, can react with water at the temperature of more than 500 ℃ to generate carbon dioxide, toxic phosgene, chlorine and hydrogen chloride gas, and can accelerate the decomposition of an ozone layer, so that the ozone layer is stopped. The use of carbon tetrachloride is strictly limited by the country, and is only used for the raw material use and special use of non-ozone depleting substances.

Disclosure of Invention

The invention aims to provide a novel method for measuring the content of the dimeticone emulsion, which has the advantages of accurate measurement, good reproducibility and relatively environment-friendly solvent.

In order to achieve the purpose, the invention is realized by the following technical scheme: the content determination method of the dimeticone emulsion comprises the following steps:

(1) preparation of a test solution: taking a proper amount (about 50mg of simethicone) of the product, precisely weighing, placing the product in a conical flask with a plug (or a screw cap), adding 50ml of 1mol/L hydrochloric acid solution, precisely adding 25ml of n-heptane, shaking for 5 minutes with force, transferring the mixture to a 125ml separating funnel, standing for 30 minutes, after layering, separating an n-heptane layer, adding 3g of anhydrous sodium sulfate, shaking, filtering, and clarifying the filtrate to obtain a sample solution.

(2) Preparation of control solutions: a dimethylpolysiloxane control (about 50mg) was weighed out precisely, and prepared in the same manner as in the test solution from the "conical flask with stopper (or cap screwed)".

(3) Preparation of a blank solution: 10ml of n-heptane is taken, 3g of anhydrous sodium sulfate is added, shaking is carried out, and the filtered clear solution is used as a blank solution.

(4) The determination method comprises the following steps: selecting 1260cm wavelength by infrared spectrophotometry^-1±2cm^-1And measuring the absorbances of the test solution and the reference solution in a 0.5mm absorption cell (HF-8 fixed liquid cell) and calculating the contents.

The beneficial technical effects of the invention are as follows: the method for measuring the content of the dimeticone emulsion has the characteristics of accurate measurement, good reproducibility and relatively environment-friendly solvent, and can be used for conventional analysis and quality control of dimeticone emulsion samples through verification.

Drawings

FIG. 1 is a linear relationship diagram of a dimethicone control;

Detailed Description

In order to verify the effect of the content determination method, the inventor carries out a large number of experiments and scientifically verifies the finally determined determination method, and the verification experiments are as follows:

system suitability test

Respectively measuring the reference solution and the sample solution for 6 times according to the content measurement method, measuring the absorbance, and inspecting the system applicability. The results of the tests are given in the following table:

TABLE 1 System suitability results

The system applicability test determines that the absorption RSD% of the reference substance and the sample solution is less than 2.0%, and meets the requirement, and the test result shows that the content determination method has good system applicability.

Blank auxiliary material interference test

Blank auxiliary materials, reference substances, raw materials and samples are respectively precisely weighed, a test solution is respectively prepared according to a test solution treatment method, the test is carried out according to a dimethicone emulsion content determination method, and the test results are shown in the following table:

TABLE 2 results of the specificity test

The test result shows that the blank solvent and the auxiliary materials have no interference to the content determination of the dimeticone, and the content determination method has good specificity.

Linear range

Taking a proper amount of simethicone reference substances, precisely weighing, preparing 20ml of stock solution of 10mg/ml, diluting with n-heptane to prepare solutions with the concentrations of about 1.0mg/ml, 1.5mg/ml, 2.0mg/ml, 2.5mg/ml and 3.0mg/ml, taking the solutions as 5 parts of solutions for linear measurement, measuring the absorbance of the solutions according to a content measurement method, and solving a linear equation of the absorbance and the concentration and a correlation coefficient. The results of the examination are shown in Table 4 below and FIG. 1;

TABLE 4 Linear Range

Linear equation of fig. 1: a-0.2482 x-0.0008 r-0.999

The test result shows that the dimeticone solution has good linearity in the concentration range of 1.0090 mg/ml-3.0269 mg/ml.

Repeatability:

taking about 50mg of simethicone working reference substance, precisely weighing, preparing reference substance solution according to the reference substance solution preparation method, and preparing 2 parts in parallel; another sample of a proper amount (about equivalent to 50mg of dimethicone) is prepared into a sample solution according to the sample solution treatment method, 6 parts are prepared in parallel, the absorbance is measured according to a content measurement method, the content of 6 parts of the solution is calculated, and the RSD (n is 6) is calculated.

TABLE 6 repeatability

The content determination result RSD of 6 samples is less than 2.0 percent by parallel determination, and the test result shows that the repeatability of the method for determining the content of the dimeticone emulsion is good.

Intermediate precision:

taking about 50mg of dimethicone reference substance by different operators (B) at different time, precisely weighing, preparing reference substance solution according to a reference substance solution preparation method, preparing 2 parts in parallel, taking a proper amount of sample (about equivalent to 50mg of dimethicone) for precise weighing, preparing test solution according to a test solution treatment method, preparing 6 parts in parallel, measuring the absorbance according to a content measurement method, calculating the content of 6 parts of solution, calculating RSD, and finally combining 6 repetitive content data (operator A measurement) to calculate the RSD of 12 content data.

TABLE 7 intermediate precision

The content measurement result RSD of 6 samples is measured in parallel by different operators at different time, the content repeatability and the intermediate precision 12 data RSD are 0.80 percent and are both less than 2.0 percent, the requirement is met, and the test result shows that the intermediate precision of the method for measuring the content of the dimeticone emulsion is good.

Accuracy (recovery):

respectively taking about 40mg, 50mg and 60mg of simethicone as reference substances, respectively, precisely weighing, respectively adding a proper amount of blank auxiliary materials (about equivalent to 50mg of simethicone), preparing a sample solution according to a sample solution treatment method, taking about 50mg of the reference substances, precisely weighing, preparing a reference substance solution according to a reference substance solution preparation method, preparing 2 parts in parallel, measuring the absorbance according to a content measurement method, and calculating the sample recovery rate.

Table 8 accuracy results the method determines that the high, medium and low concentration content recovery rates are all between 98% and 105%, the average recovery rate is 101.92%,

RSD is less than 2.0%; the method meets the requirements, and the test result shows that the method for determining the content of the dimeticone emulsion has high accuracy and good recovery rate.

Durability test

Taking a reference solution and a test solution, and respectively inspecting the shaking time of the sample, the dosage of the dehydrating agent of the sample and the scanning times according to a content measurement method. The results of the tests are given in the following table:

TABLE 9 durability test results

And (4) conclusion: the RSD of the content determination data under different test conditions is not more than 2.0 percent, the requirement is met, and the test result shows that the durability of the method for determining the content of the dimeticone is good.

Stability of the solution

Taking about 50mg of simethicone working reference substance, precisely weighing, preparing reference substance solution according to the reference substance solution preparation method, and preparing 2 parts in parallel; taking a proper amount of sample (about equivalent to 50mg of dimeticone) to prepare a sample solution according to a sample solution treatment method, preparing 2 parts in parallel, storing at room temperature for 0, 2, 4, 8 and 24 hours, using a freshly prepared standard solution as a reference at each interval point, measuring the stored sample solution and the reference solution according to a content measurement method, and calculating the absorbance of the sample solution and the reference solution.

The results of the tests are given in the following table:

TABLE 10 stability test results of the solutions

Time (h)	Control content (%)	Content of test sample (%)
			0	100.00	97.67
2	100.09	98.16
			4	100.89	98.41
8	101.06	98.12
			24	100.39	97.31
RSD(％)	0.47	0.45
			Content Change (%)	Stabilization	Stabilization

And (4) conclusion: the relative standard deviation of the content of the reference substance solution is less than or equal to 2.0 percent; the content of the test solution is within the range of 90.0-110.0%, and the relative standard deviation of the content is less than or equal to 2.0%, which represents the reference solution; the test solution is stable over this period of time.

Taking 3 batches of simethicone emulsion, preparing a sample solution by a method before and after changing, and performing content determination by an infrared spectrophotometry. The content of the simethicone emulsion before changing is 105.86%, 102.08% and 103.52% respectively; the modified content method comprises 105.94%, 103.52% and 103.34% of the three simethicone emulsion; the results were indistinguishable.