CN110907543A - Experimental method for adsorbing bile acid of hydrotalcite chewable tablet - Google Patents
Experimental method for adsorbing bile acid of hydrotalcite chewable tablet Download PDFInfo
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Abstract
The invention provides an experimental method for adsorbing bile acid of a hydrotalcite chewable tablet, which is characterized in that 0.1mol/l hydrochloric acid solution is respectively added into the hydrotalcite chewable tablet, the hydrochloric acid solution contains 0.5mmol/l bile acid salt, the mixture is uniformly mixed, the obtained solution is cultured for 1 hour at 37 +/-0.5 ℃, then the solution is centrifuged for 15 minutes at 2000rpm, and the supernatant is filtered, thus obtaining the hydrotalcite chewable tablet; meanwhile, the method is operated without adding the aluminum magnesium carbonate to be used as a reference solution, a 0.1mol/l hydrochloric acid solution aluminum magnesium carbonate sample without containing bile acid salt is added to be used as a blank sample solution, and after the high performance liquid chromatography method is adopted for determination, the adsorption rate is calculated according to the peak areas of the unadsorbed bile acid in the reference solution and the supernate of the test solution. The method can determine the adsorption condition of hydrotalcite chewable tablet on bile acid salt, and has good durability and convenient determination.
Description
Technical Field
The invention relates to a detection method, in particular to a method for determining bile acid salt adsorption of a hydrotalcite chewable tablet.
Background
The hydrotalcite chewable tablet is mainly used for treating chronic gastritis and stomach discomfort symptoms related to gastric acid, such as stomachache, heartburn (heartburn), acid eructation, satiety and the like. The hydrotalcite is an antacid and anti-bile gastric mucosa protective agent, can directly act on a pathological change part, can quickly improve and relieve gastric diseases, quickly neutralize gastric acid, keep for a long time, prevent pepsin from damaging the stomach, protect the gastric mucosa and quickly relieve the uncomfortable symptoms of the stomach.
Bile acid is an important component of bile and plays an important role in fat metabolism. Normally, the gastric juice does not contain bile acid, and the gastric acid does not change the bile acid. However, it has been found that in the pathogenesis of gastric ulcer, bile acid flows back from the duodenum to the stomach, causing damage to the gastric mucosa, and bile acid flow back promotes the stomach to become cancerous.
At present, USP, BP, EP, Chinese pharmacopoeia and national drug standards do not record a method for detecting bile acid, and no relevant regulation is carried out on an hydrotalcite chewable tablet bile acid adsorption test. In order to ensure the research, development and production quality of the hydrotalcite chewable tablet, an experimental method for adsorbing bile acid of the hydrotalcite chewable tablet is obtained through research.
Disclosure of Invention
Aiming at the defects, the invention aims to provide an experimental method for adsorbing bile acid of the hydrotalcite chewable tablet.
The invention relates to an experimental method for adsorbing bile acid of a magnesium aluminate chewable tablet, which comprises the following steps:
pretreatment: grinding 20 tablets of the product, sieving by a No. 5 sieve, precisely weighing 1/20 with average tablet weight, adding 5ml of 0.1mol/l hydrochloric acid solution containing 0.5m mol/l bile acid salt, mixing uniformly by vortex, culturing the obtained solution at 37 +/-0.5 ℃ for 1 hour, shaking uniformly during the culture process, and centrifuging at 2000rpm for 15 minutes; meanwhile, the method is operated without adding aluminum and magnesium carbonate to be used as a reference solution; and calculating the adsorption rate according to the peak areas of unadsorbed bile acid in the control solution and the test solution.
The chromatographic method comprises the following steps: mobile phase: methanol-acetonitrile-0.05 mol/l phosphate buffer (40:40:50), pH adjusted to 3.0 with phosphoric acid, sample amount: 20ul, column temperature: at 30 ℃, the flow rate was: 1.0ml/min, wavelength: 200nm, and the chromatographic column comprises: octadecyl bonded silica gel is used as a filler.
Calculating the formula:
the beneficial technical effects of the invention are as follows: the method adopts the high performance liquid chromatography, has simple and convenient operation, good specificity and high accuracy, and can effectively control the bile acid adsorption condition of the hydrotalcite chewable tablet.
Drawings
In fig. 1, the numbers 1, 2, 3, 4, and 5 are 20%, 50%, 80%, 100%, and 200% mixed controls, respectively.
Detailed Description
Example 1
In order to determine the bile acid adsorption of the hydrotalcite chewable tablet, the invention provides an experimental method for the bile acid adsorption of the hydrotalcite chewable tablet. In the technical scheme, the pretreatment method of the experiment is determined by selecting a medium and the volume of the medium, and determining the type and concentration of the bile acid salt. Then, according to a comparative study on the adsorption of bile acid outside the hydrotalcite chewable tablet (Chin Pharm J, No. 11, volume 35, 11, 2000navember. Vol.35No11, 11, 2000J. pharmaceutical journal of China), chromatographic conditions are optimized, and finally, an experimental method for the adsorption of bile acid on the hydrotalcite chewable tablet is determined.
In the following embodiments, the drugs, reagents and instruments used are shown in tables 1, 2 and 3:
TABLE 1 sample information
TABLE 2 control information
| Name (R) | Batch number | Specification of | Content (wt.) | Origin of origin |
| Taurocholic acid sodium salt | L780Q19 | 1G | 98％ | Bailingwei-medicine |
| Glycocholic acid sodium salt | 1-CYJ-2-2 | 1G | 98％ | TRC |
| Sodium taurochenodeoxycholate | 29-GHZ-67-1 | 1G | 95％ | TRC |
| Deoxycholic acid sodium cholate | 1-NYL-90-1 | 1G | 95％ | TRC |
| Glycine sodium deoxycholate | 5-YFD-138-1 | 1G | 95％ | TRC |
TABLE 3 Main Instrument information
Selection of medium:
the medical science considers that the pH value of gastric acid is about 0.9-1.2 (about equivalent to the pH value of 0.1mol/l hydrochloric acid solution), the main component of the gastric acid is hydrochloric acid and also contains pepsin, and the gastric acid is prepared by dilute hydrochloric acid and pepsin in artificial gastric juice in pharmacopoeia; therefore, 0.1mol/l hydrochloric acid and artificial gastric juice can be selected in the bile acid adsorption test.
Selection of the volume of the medium:
the normal human gastric acid amount is 20ml to 100ml, the average is 50ml, and patients with gastric hyperacidity are generally 100ml to 150ml, therefore, the medium volume is selected to be 100ml in the test.
Determination of bile acid salt species:
according to the chemical structure division, bile acid can be divided into free bile acid and combined bile acid, and the free bile acid comprises cholic acid, deoxycholic acid and chenodeoxycholic acid; free bile acids are unstable in acid and Ca2+The bound cholic acid is mainly the product of free cholic acid bound with glycine or taurine, including glycocholic acid and taurocholateCholic acid, glycochenodeoxycholic acid, taurochenodeoxycholic acid, glycodeoxycholic acid, taurodeoxycholic acid, conjugated bile acid, stable in acid and Ca2+The compound is not easy to precipitate in existence and is a main substance which damages gastric mucosa in bile reflux, so that combined bile acid is selected for carrying out adsorption test research on hydrotalcite;
according to medical analysis and reference literature, "high pressure liquid chromatography for bile-bound bile acid quantitation (1990, 7, 4) in the journal of experimental surgery of china), the dissolution of each cholate, i.e., 0.1mol/l hydrochloric acid solution of glycine-ammonia cholate or the solubility of artificial gastric juice is poor, and particularly, sodium glycodeoxycholate is hardly dissolved in 0.1mol/l hydrochloric acid solution or artificial gastric juice, so sodium glycodeoxycholate is not selected in this study, and the selected bound bile acid salts include: sodium taurocholate, sodium glycocholate, sodium taurochenodeoxycholate, sodium glycochenodeoxycholate, and sodium taurodeoxycholate.
Selection of the using amount of the aluminum magnesium carbonate:
the dosage of the tablet with the specification of 0.5g is 1-2 tablets, the minimum dosage of one time, namely 1 tablet respectively, is selected during screening by the experimental chromatographic method, and 1 tablet of hydrotalcite is tested during research on the tablet with the specification of 0.5 g.
Determination of bile acid salt concentration:
refer to the foreign document A COMPARATIVE ASSESSMENT OF A NEW ANTACID FORMATIONBASED ON MAGLDARDITE (Journal OF Clinical and Hospital Pharmacy (1983)8,349-355), wherein in the antacid bile salt adsorption test, the concentration OF bile salt is selected to be 0.5mmol/l (molecular weight is about 500), i.e., 0.25 mg/ml. Therefore this concentration was chosen for the experiments in this study.
A pretreatment process:
the preliminary in vitro test method for determining the product comprises the following steps: adding appropriate amount (containing 0.5g hydrotalcite) into 100ml 0.1mol/l hydrochloric acid solution containing 0.5m mol/l bile acid salt, culturing at 37 + -0.5 deg.C for 1 hr, shaking, and centrifuging at 2000rpm for 15 min; sample solutions of five bile acid salts including sodium taurocholate, sodium glycocholate, sodium taurodeoxycholate and sodium glycochenodeoxycholate are prepared in the same way respectively. Meanwhile, the method is operated without adding aluminum and magnesium carbonate to be used as a reference solution; and calculating the adsorption rate according to the peak areas of unadsorbed bile acid in the control solution and the test solution.
By referring to the dosage of the antacid in the bile acid salt adsorption literature reported abroad, the volume of the hydrotalcite and the hydrochloric acid is reduced by 20 times in the same proportion on the basis of the method, namely the method is modified as follows: adding appropriate amount (about 25mg magnesium aluminum carbonate) into 5ml 0.1mol/l hydrochloric acid solution containing 0.5m mol/l bile acid salt, culturing the above obtained solution at 37 + -0.5 deg.C for 1 hr, shaking and mixing, and centrifuging at 2000rpm for 15 min; meanwhile, the method is operated without adding aluminum and magnesium carbonate to be used as a reference solution; and calculating the adsorption rate according to the peak areas of unadsorbed bile acid in the control solution and the test solution.
Optimization of chromatographic conditions:
according to various literatures at home and abroad, the experiment is optimized according to comparative research on adsorption of cholic acid outside a hydrotalcite chewable tablet (Chin Pharm J, 11 th No. 11, volume 35, 2000 naveman. Vol.35No11, 2000) in the reference literature, and the chromatographic method is determined.
The specific conditions are as follows: mobile phase: methanol-acetonitrile-0.03 mol/l phosphate buffer (40:40:50), pH adjusted to 3.0 with phosphoric acid, sample amount: 20ul, column temperature: at 30 ℃, the flow rate was: 1.0ml/min, chromatographic column: diamonsil C185um, 150 × 4.6mm, run time: and (5) 25 min.
The specific process is as follows:
1. preparation of the solution
Blank solvent: taking 9.0ml of hydrochloric acid solution, adding water to dilute the hydrochloric acid solution to 1000ml, and preparing 0.1mol/l hydrochloric acid solution;
preparation of control solution: weighing appropriate amount (about 12.5mg) of bile acid salt reference substance, precisely weighing, respectively placing into 50ml measuring bottles, adding 0.1mol/l hydrochloric acid solution to dissolve and dilute into 0.25mg/ml (0.5mmol/l, molecular weight about 500) of reference solution, respectively as reference solution;
preparation of mixed control solution: an appropriate amount (about 12.5mg) of each bile acid salt reference substance is weighed respectively, precisely weighed, placed in a 50ml measuring flask, dissolved by adding 0.1mol/l hydrochloric acid solution and diluted into a control solution of 0.25mg/ml (0.5mmol/l, molecular weight about 500) to serve as a mixed control solution.
Preparing a sample solution: taking the hydrotalcite chewable tablet (about 25mg hydrotalcite), respectively adding 5ml of 0.1mol/l hydrochloric acid solution containing 0.5mmol/l bile acid salt, culturing the obtained solution at 37 +/-0.5 ℃ for 1 hour, shaking uniformly during the culture process, centrifuging at 2000rpm for 15 minutes, and filtering to obtain the product.
2. Selection of wavelength
Five single bile acid salt controls were prepared to contain about 0.075mg of solution per 1ml and uv-scanned by uv-visible spectrophotometry (0401 in the four parts of the chinese pharmacopoeia 2015). The test result shows that: sodium taurocholate, sodium glycocholate, sodium deoxycholic acid, sodium taurochenodeoxycholate and sodium glycochenodeoxycholate have maximum absorption at a wavelength of 199nm, so that a detection wavelength of 200nm is selected preliminarily.
3. Selection of mobile phase salt solution concentration
The concentrations of 0.02M, 0.03M, 0.04M, 0.05M and 0.06M were selected for the test, and the specific values are shown in Table 4.
Table 4 comparison of different mobile phase salt concentration results
| Concentration (M) | Minimum degree of separation | Tailing factor | Last peak retention time | Number of theoretical plate |
| 0.02 | 1.2 | 1.0～2.2 | 18.521 | 2500～5700 |
| 0.03 | 2.4 | 0.9～1.8 | 22.558 | 3000～5400 |
| 0.04 | 2.4 | 0.9～1.6 | 19.055 | 3200～6000 |
| 0.05 | 2.5 | 0.9～1.4 | 19.043 | 3500～5700 |
| 0.06 | 2.6 | 1.0～1.5 | 18.809 | 4000～6200 |
As can be seen from the above table, when the concentration of the buffer salt is 0.05M, the values of the respective parameters of the chromatographic peak are better, and it is preliminarily determined that the concentration of the buffer salt is 0.05M.
4. Selection of pH of mobile phase
The pH values were adjusted to 2.5, 3.5 and 4.0 with phosphoric acid, respectively, as shown in Table 5.
TABLE 5 comparison of pH results for different mobile phases
| pH value | Minimum degree of separation | Tailing factor | Last peak retention time | Number of theoretical plate |
| 2.5 | Is not separated | 0.9～2.0 | About 20min | 3000～5000 |
| 3.0 | 2.4 | 0.9～1.8 | 22.558 | 3000～5400 |
| 3.5 | 2.4 | 0.9～2.1 | 20.163 | 3000～5900 |
| 4.0 | 2.3 | 0.9～1.9 | 19.391 | 3000～5600 |
As can be seen from the above table, the change of the pH value has little influence on each parameter of the chromatographic peak; simultaneously, the pH value change test is carried out on the other three chromatographic columns, and the result change is consistent with that of the No. 91 chromatographic column; thus a pH of 3.0 was chosen.
The experimental chromatographic conditions were finally determined as follows:
mobile phase: methanol-acetonitrile-0.05 mol/l phosphate buffer (40:40:50), pH adjusted to 3.0 with phosphoric acid, sample amount: 20ul, column temperature: at 30 ℃, the flow rate was: 1.0ml/min, wavelength: 200nm, and the chromatographic column comprises: octadecyl bonded silica gel is used as a filler.
Optimization of pretreatment
1. Selection and preparation method of control
The dissolution of the single control and the mixed control in two media of 0.1mol/l hydrochloric acid and artificial gastric juice is respectively tested, and the following phenomena occur:
① adopts 0.1mol/L hydrochloric acid solution (pH value is about 0.9-1.2) as medium, sodium glycocholate in five kinds of bile acid salts (sodium taurocholate, sodium glycocholate, sodium taurochenodeoxycholate, sodium taurodeoxycholate and sodium glycochenodeoxycholate) can only dissolve about 90% in 0.1mol/L hydrochloric acid medium, and sodium glycochenodeoxycholate can only dissolve about 50%.
② artificial gastric juice (pH about 1.6) is prepared as medium, and the dissolution degree of the five bile acid salts is basically consistent with that of hydrochloric acid solution (pH value about 0.9-1.2) of 0.1 mol/L.
③ considering whether partial bile acid salt is not dissolved due to saturation of bile acid salt solution, experiments were carried out by preparing sodium glycochenodeoxycholate with different concentrations, and it was found that sodium glycochenodeoxycholate was dissolved only by about 50% even though the concentration was reduced by 10 times.
④ considering whether the dissolution of bile acid salts is affected by pH, it was found that sodium glycochenodeoxycholate can be dissolved in hydrochloric acid solutions prepared at pH values of 3.0, 3.5 and 4.2, and that sodium glycochenodeoxycholate can be completely dissolved at pH 3.0.
It follows that the solubility of bile acid salts (especially glycocholate) is related to the pH of the dissolution medium. The pH value of the bile acid salt is 1-2, and the solubility of the bile acid salt in artificial gastric juice and 0.1mol/L hydrochloric acid solution is not good.
Because the solubility of the single control and the mixed control is low, the controls are filtered separately, and after standing for 1-2h, the mixed control precipitates out. After the 200% mixed control solution is diluted to 100%, 80%, 50%, 20% solution and left for 1-2 hours, the precipitate is sucked out, and the result is shown in picture 1.
The linearity and recovery rate test is carried out, 0.1mol/L hydrochloric acid solution is used as a medium solvent, and the test results are shown in Table 6:
table 6 results of linear tests (R) for single and mixed bile salts2)
As can be seen from the table, the precipitate adsorbed after mixing was sodium glycochenodeoxycholate, and after filtration, linear R2 reached only 0.93
TABLE 7 recoverability test results for single bile acid salts and mixed bile acid salts
As is clear from the table, the precipitate adsorbed after mixing was sodium glycochenodeoxycholate, and the higher the concentration of the preparation, the more the precipitate was aspirated, and after filtration, the average values of the absolute recovery of 80%, 50%, and 20% were larger in 100% control, and the RSD value was also larger.
According to the above test, a single control was finally selected for the experiment.
2. The medium is artificial gastric juice or 0.1mol/L hydrochloric acid solution for screening.
The experimental results are as follows:
TABLE 8 comparison of bile acid adsorption results with different media
As can be seen from the table, the adsorption values of the five bile acid salts are not obviously different from the adsorption value of the medium of 0.1mol/L hydrochloric acid.
In the experimental process, because the artificial gastric juice is thick, the filtration is performed twice, namely the vacuum filtration and the needle type filter filtration, and the operation is not convenient. And finally, selecting 0.1mol/L hydrochloric acid solution as the medium.
Claims (2)
1. An experimental method for adsorbing bile acid of a magnesium hydrotalcite chewable tablet is characterized by comprising the following steps: the method comprises the following steps:
1) grinding hydrotalcite chewable tablets, sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l bile acid salt, mixing uniformly in a vortex manner, culturing the obtained solution at 37 +/-0.5 ℃ for 1 hour, shaking uniformly in the culture process, centrifuging the solution of hydrochloric acid at 2000rpm for 15 minutes, mixing uniformly in a vortex manner, culturing the obtained solution at 37 +/-0.5 ℃ for 1 hour, shaking uniformly in the culture process, and centrifuging at 2000rpm for 15 minutes to obtain a test solution 1;
2) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l sodium taurocholate, and mixing uniformly in a vortex manner to prepare a test solution 2;
3) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l sodium glycocholate, and mixing uniformly in a vortex manner to prepare a test solution 3;
4) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l sodium taurochenodeoxycholate, and mixing uniformly in a vortex manner to prepare a test solution 4;
5) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l sodium taurodeoxycholate, and mixing uniformly in a vortex manner to prepare a test solution 5;
6) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid and 0.5m mol/l sodium glycochenodeoxycholate, and mixing uniformly in a vortex manner to prepare a test solution 6;
7) grinding the hydrotalcite chewable tablets by adopting the same method in the step 1), sieving, weighing 1/20, adding 5ml of 0.1mol/l hydrochloric acid solution, and mixing uniformly in a vortex manner to prepare a reference solution;
8) the adsorption rate was calculated by HPLC method using the areas of the peaks of the bile acids not adsorbed in the supernatants of the control solution and the test solutions 1, 2, 3, 4, 5, 6.
2. The experimental method for bile acid adsorption of hydrotalcite chewable tablet according to claim 1, wherein: the chromatographic conditions for HPLC chromatography were:
mobile phase: methanol-acetonitrile-0.05 mol/l phosphate buffer (40:40:50), pH adjusted to 3.0 with phosphoric acid, sample amount: 20ul, column temperature: at 30 ℃, the flow rate was: 1.0ml/min, wavelength: 200nm, and the chromatographic column comprises: octadecyl bonded silica gel is used as a filling agent;
calculating the formula:
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0379161A2 (en) * | 1989-01-20 | 1990-07-25 | Hoechst Aktiengesellschaft | Use of alkylated polyethyleneimines as therapeutic agent adsorbing bile acid and pharmaceutical compositions thereof |
-
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0379161A2 (en) * | 1989-01-20 | 1990-07-25 | Hoechst Aktiengesellschaft | Use of alkylated polyethyleneimines as therapeutic agent adsorbing bile acid and pharmaceutical compositions thereof |
Non-Patent Citations (4)
| Title |
|---|
| D. F. MCCAFFERTY 等: "A COMPARATIVE ASSESSMENT OF A NEW ANTACID FORMULATION BASED ON MAGALDRATE", 《JOURNAL OF CLINICAL AND HOSPITAL PHARMACY》 * |
| 刘萍 等: "芋头多糖提取工艺优化及其体外结合脂类和胆酸盐能力研究", 《食品与机械》 * |
| 叶敏 等: "铝碳酸镁咀嚼片体外吸附胆酸的比较研究", 《中国药学杂志》 * |
| 石景森 等: "胆汁中结合胆汁酸高压液相色谱定量分析", 《陕西医学杂志》 * |
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Application publication date: 20200324 |