Method for detecting content of arsenic in quick-acting calculus bovis pill and application of quick-acting calculus bovis pill

Abstract

The invention relates to a method for detecting the content of arsenic in quick-acting calculus bovis pills and application thereof, and belongs to the technical field of traditional Chinese medicine detection. The invention provides a method for detecting the content of arsenic in quick-acting bezoar pills, which comprises the following steps: mixing the quick-acting bezoar pills, nitric acid and hydrochloric acid, digesting, and adding water to a constant volume to obtain a diluent; mixing the acid solution and the diluent to obtain a sample solution; and measuring the absorbance of the sample solution by adopting an atomic absorption spectrophotometric method, and calculating the content of arsenic in the quick-acting calculus bovis pill according to the standard curve. The detection method provided by the invention can accurately detect the content of arsenic in the quick-acting calculus bovis pill, and has the characteristics of high specificity, repeatability, stability and accuracy.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for detecting the arsenic content in Suxiao Niuhuang Wan and an application thereof. Background Art

[0002] The Quick-Acting Niuhuang Pill is included in the "Chinese Pharmacopoeia". It is a large honey pill with a fragrant smell, slightly bitter taste, and yellow-brown to brown color. It has the effects of clearing away heat and detoxifying, opening the orifices and calming the nerves. It can be used to treat irritability and coma caused by internal phlegm and fire, and dizziness caused by hypertension.

[0003] Realgar, a component of Suxiao Niuhuang Wan (Bulrush Pills), has the properties of dispersing heat, warming, and removing dampness, as well as removing phlegm, and detoxifying. Its main component is arsenic disulfide (As2S2), indicating that Suxiao Niuhuang Wan (Bulrush Pills) contain arsenic, a harmful element. Therefore, to better control the quality of Suxiao Niuhuang Wan (Bulrush Pills), quantitative testing of their arsenic content is necessary.

[0004] However, the existing technology for detecting the arsenic content of Suxiao Niuhuang Wan has defects such as low accuracy and poor stability, and cannot provide a reference basis for the drug quality control of Suxiao Niuhuang Wan. Summary of the Invention

[0005] The purpose of the present invention is to provide a method for detecting the arsenic content in Suxiao Niuhuang Wan and its application, so as to solve the problems of low accuracy and poor stability in the existing method for detecting the arsenic content in Suxiao Niuhuang Wan.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for detecting the arsenic content in Suxiao Niuhuang Wan, comprising the following steps:

[0008] (1) mixing Suxiao Niuhuang Wan, nitric acid and hydrochloric acid to obtain a mixed solution; digesting the mixed solution to obtain a digestion solution; adding water to the digestion solution to make the volume to 50 mL to obtain a dilution solution;

[0009] (2) mixing nitric acid, hydrochloric acid and water to obtain an acid solution; mixing the acid solution and a diluent to obtain a sample solution;

[0010] (3) The absorbance of the sample solution was determined by atomic absorption spectrophotometry, and the arsenic content in the Suxiao Niuhuang Wan was calculated based on the standard curve;

[0011] The digestion process in step (1) is as follows: The mixed solution is heated from 30°C to 120°C and then maintained at 120°C for 5 - 15 minutes; then heated from 120°C to 160°C and maintained at 160°C for 10 - 20 minutes; then heated from 160°C to 180°C and maintained at 180°C for 25 - 45 minutes; finally cooled from 180°C to 30°C to obtain the digested solution.

[0012] Preferably, the mass - to - volume ratio of the rapid - effect bezoar - containing pill and nitric acid in step (1) is 0.05 - 0.3 g: 3 - 6 mL;

[0013] The mass - to - volume ratio of the rapid - effect bezoar - containing pill and hydrochloric acid is 0.05 - 0.3 g: 0.5 - 2 mL.

[0014] Preferably, the digestion method in step (1) is microwave digestion, and the power of the digestion is 750 - 1500 W.

[0015] Preferably, the volume ratio of nitric acid, hydrochloric acid and water mixed in step (2) is 3 - 6: 0.5 - 2: 42 - 46.5;

[0016] The volume ratio of the acid solution and the diluent mixed is 40 - 50: 4 - 7.

[0017] Preferably, the wavelength of the measurement in step (3) is 193.7 nm.

[0018] Preferably, the rapid - effect bezoar - containing pill comprises the following components in parts by mass: artificial bezoar 15 - 30 parts, concentrated powder of buffalo horn 40 - 60 parts, Coptis chinensis 20 - 40 parts, Scutellaria baicalensis 10 - 30 parts, Gardenia jasminoides 10 - 30 parts, borneol 3 - 10 parts, Curcuma aromatica 15 - 35 parts, cinnabar 10 - 35 parts, realgar 15 - 30 parts, Acorus tatarinowii 15 - 35 parts, mother - of - pearl 20 - 40 parts, refined honey 173 - 375 parts.

[0019] The present invention also provides the application of the above - mentioned method in accurately detecting the arsenic content in the rapid - effect bezoar - containing pill.

[0020] The present invention has the following technical effects and advantages:

[0021] The present invention uses atomic absorption spectrophotometry to quantitatively analyze the arsenic element in the rapid - effect bezoar - containing pill, which has the characteristics of high specificity, repeatability, stability and accuracy, can provide guarantee for the safety of clinical medication, and at the same time provide a basis for formulating the quality standard of the arsenic element content in the rapid - effect bezoar - containing pill. Detailed implementation manners

[0022] The present invention provides a method for detecting the arsenic content in the rapid - effect bezoar - containing pill, which comprises the following steps:

[0023] (1) Mix the Suxiao Niuhuang Pills, nitric acid, and hydrochloric acid to obtain a mixed solution; digest the mixed solution to obtain a digested solution; add water to the digested solution to make up the volume to 50 mL to obtain a diluted solution.

[0024] (2) Mix nitric acid, hydrochloric acid, and water to obtain an acid solution; mix the acid solution and the diluted solution to obtain a sample solution.

[0025] (3) Use atomic absorption spectrophotometry to measure the absorbance of the sample solution, and calculate the arsenic content in the Suxiao Niuhuang Pills according to the standard curve.

[0026] The process of digestion described in step (1) is as follows: After heating the mixed solution from 30 °C to 120 °C, maintain it at 120 °C for 5 - 15 min, preferably 10 min; then heat it from 120 °C to 160 °C, and maintain it at 160 °C for 10 - 20 min, preferably 15 min; then heat it from 160 °C to 180 °C, and maintain it at 180 °C for 25 - 45 min, preferably 30 min; finally, cool it from 180 °C to 30 °C to obtain the digested solution.

[0027] In the present invention, the mass - volume ratio of the Suxiao Niuhuang Pills and nitric acid in step (1) is 0.05 - 0.3 g: 3 - 6 mL, preferably 0.2 g: 4 mL.

[0028] The mass - volume ratio of the Suxiao Niuhuang Pills and hydrochloric acid in step (1) is 0.05 - 0.3 g: 0.5 - 2 mL, preferably 0.2 g: 1 mL.

[0029] In the present invention, the digestion method in step (1) is microwave digestion, and the digestion power is 750 - 1500 W, preferably 1000 W.

[0030] In the present invention, the volume ratio of nitric acid, hydrochloric acid, and water in step (2) is 3 - 6: 0.5 - 2: 42 - 46.5, preferably 4: 1: 45.

[0031] The volume ratio of the acid solution and the diluted solution in step (2) is 40 - 50: 4 - 7, preferably 45: 5.

[0032] In the present invention, the wavelength of the measurement in step (3) is 193.7 nm.

[0033] In the present invention, the quick-acting Niuhuang Pills comprise the following components in parts by mass: artificial cow-bezoar 15 - 30 parts, preferably 25 parts; concentrated powder of buffalo horn 40 - 60 parts, preferably 50 parts; Coptis chinensis 20 - 40 parts, preferably 25 parts; Scutellaria baicalensis 10 - 30 parts, preferably 25 parts; Gardenia jasminoides 10 - 30 parts, preferably 25 parts; borneol 3 - 10 parts, preferably 5 parts; Curcuma aromatica 15 - 35 parts, preferably 25 parts; cinnabar 10 - 35 parts, preferably 25 parts; realgar 15 - 30 parts, preferably 25 parts; Acorus tatarinowii 15 - 35 parts, preferably 25 parts; mother-of-pearl 20 - 40 parts, preferably 25 parts; refined honey 173 - 375 parts, preferably 280 parts.

[0034] In the present invention, the preparation method of the quick-acting Niuhuang Pills is as follows: after pulverizing artificial cow-bezoar, Coptis chinensis, Scutellaria baicalensis, Gardenia jasminoides, borneol, Curcuma aromatica, cinnabar, realgar, Acorus tatarinowii, and mother-of-pearl, mix them with the concentrated powder of buffalo horn and sieve to obtain traditional Chinese medicine powder; mix the traditional Chinese medicine powder and refined honey to obtain the quick-acting Niuhuang Pills.

[0035] In the present invention, the particle size of the traditional Chinese medicine powder is 120 - 180 μm, preferably 150 μm.

[0036] The present invention also provides the application of the above method in accurately detecting the arsenic content in the quick-acting Niuhuang Pills.

[0037] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0038] In the reagents of the present invention, the single-element arsenic standard solution comes from the National Center for Analysis and Testing of Nonferrous Metals and Electronic Materials;

[0039] In the instruments of the present invention, the TAS-990 atomic absorption spectrophotometer is purchased from Beijing Purkinje General Instrument Co., Ltd.

[0040] Example 1: Detection method for the arsenic content in the quick-acting Niuhuang Pills

[0041] (1) Preparation of the quick-acting Niuhuang Pills: Take 25 g of artificial cow-bezoar, 25 g of Coptis chinensis, 25 g of Scutellaria baicalensis, 25 g of Gardenia jasminoides, 5 g of borneol, 25 g of Curcuma aromatica, 25 g of cinnabar, 25 g of realgar, 25 g of Acorus tatarinowii, and 25 g of mother-of-pearl, pulverize them, mix with 50 g of the concentrated powder of buffalo horn and sieve to obtain traditional Chinese medicine powder with a particle size of 150 μm; mix the traditional Chinese medicine powder and 280 g of refined honey to make pills to obtain the quick-acting Niuhuang Pills;

[0042] (2) Preparation of standard solution: Mix 4 mL of nitric acid, 1 mL of hydrochloric acid and 45 mL of water to obtain an acid solution; dilute the single-element arsenic standard solution with the acid solution to standard solutions with arsenic concentrations of 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, and 100 μg / mL respectively, and use the acid solution as the blank solution;

[0043] (3) Plotting of standard curve: Refer to the atomic absorption spectrophotometry disclosed in the Chinese Pharmacopoeia (2020 Edition), measure the absorbance of each standard solution and the blank solution at 193.7 nm, and plot the standard curve with the absorbance as the ordinate and the arsenic concentration in each standard solution as the abscissa;

[0044] (4) Preparation of sample solution: Take 0.2 g of the quick-acting Niuhuang Pills prepared in step (1), mix it with 4 mL of nitric acid and 1 mL of hydrochloric acid to obtain a mixed solution, then place it in a polytetrafluoroethylene digestion tank, and use a microwave digester to carry out digestion under the condition of a power of 1000 W. The digestion process is as follows: heat the mixed solution from 30 °C to 120 °C, and keep it at 120 °C for 10 min; then heat it from 120 °C to 160 °C, and keep it at 160 °C for 15 min; then heat it from 160 °C to 180 °C, and keep it at 180 °C for 30 min; finally, cool it from 180 °C to 30 °C to obtain a digestion solution; dilute the digestion solution to 50 mL with water to obtain a dilution solution; take 5 mL of the dilution solution and mix it evenly with 45 mL of the acid solution prepared in step (2) to obtain a sample solution;

[0045] (5) Determination of arsenic content: Use atomic absorption spectrophotometry, use a TAS-990 type atomic absorption spectrophotometer to measure the absorbance of the sample solution at 193.7 nm, and calculate the arsenic content in the quick-acting Niuhuang Pills according to the standard curve.

[0046] Experimental Example 1: Investigation of linear relationship

[0047] Prepare the standard solution and the blank solution by the method described in step (2) of Example 1, measure and plot the standard curve by the method described in step (3) of Example 1, and plot it 3 times in total. The regression equation of the standard curve is shown in Table 1.

[0048] Table [1] Regression equation of standard curve

[0049] Frequency Regression equation R The first time y = 289610.1428x - 649.3186 0.9999 The second time y = 253846.3144x - 2092.3324 0.9995 The third time y = 247094.4612x - 1744.4115 0.9993

[0050] The results show that there is a good linear correlation between the arsenic concentration in the standard solution and the absorbance in the range of 5-100 μg / mL, and the correlation coefficient of the regression equation of the standard curve y = 289610.1428x - 649.3186 is the highest (R = 0.9999). Therefore, the arsenic content in the quick-acting Niuhuang Pills is calculated using this standard curve.

[0051] Experimental Example 2: Negative Interference Experiment

[0052] The rapid-acting bezoar pill without realgar was prepared by the method described in step (1) of Example 1 as a negative control. The negative control sample solution was prepared by the method described in step (4) of Example 1, and the arsenic content in the negative control sample solution was determined by the method described in Example 1, and the determination was repeated 6 times.

[0053] The results showed that arsenic was not detected in the rapid-acting bezoar pill without realgar, that is, except for realgar in the rapid-acting bezoar pill, the other traditional Chinese medicine raw materials did not interfere with the detection of arsenic content, indicating that the detection method of the present invention has good specificity.

[0054] Experimental Example 3: Repeatability Test

[0055] Twelve samples, each weighing 0.2 g, were selected from the rapid-acting bezoar pill with batch number 20241101 prepared by the method described in step (1) of Example 1. The absorbance of each sample was measured by the method described in Example 1, and the arsenic content in each sample was calculated according to the regression equation of the standard curve y = 289610.1428x - 649.3186. The results are shown in Table 2.

[0056] Table 2 Results of Repeatability Test for Arsenic Content in Rapid-Acting Bezoar Pill

[0057]

[0058]

[0059] The results showed that in the detection method of the present invention, the RSD of the repeatability test was 1.419%, indicating that the detection method of the present invention has good repeatability.

[0060] Experimental Example 4: Stability Test

[0061] Take 0.2 g of the sample from the rapid-acting bezoar pill with batch number 20241101 prepared in Experimental Example 3, and place it for 0 h, 2 h, 4 h, 8 h, 12 h, and 24 h respectively. The absorbance of each sample was measured by the method described in Example 1, and the arsenic content in each sample was calculated according to the regression equation of the standard curve y = 289610.1428x - 649.3186. The results are shown in Table 3.

[0062] Table 3 Results of Stability Test for Arsenic Content in Rapid-Acting Bezoar Pill

[0063]

[0064] The results show that in the detection method of the present invention, the RSD of the stability test is 2.653%, indicating that the detection method of the present invention has good stability.

[0065] Experimental Example 5: Standard addition recovery test

[0066] Take 12 samples from the quick-acting bezoar pills with batch number 20241101 prepared in Experimental Example 3, each about 0.2 g, add 2 mL of arsenic single-element standard solution (1000 μg / mL) respectively, mix well, measure the absorbance of each sample according to the method described in Example 1, and calculate the arsenic content in each sample according to the regression equation of the standard curve y = 289610.1428x - 649.3186. The results are shown in Table 4.

[0067] Table 4 Results of the standard addition recovery test of quick-acting bezoar pills

[0068]

[0069]

[0070] The results show that in the detection method of the present invention, the RSD of the standard addition recovery test is 3.068%, indicating that the detection method of the present invention has good accuracy.

[0071] As can be seen from the above examples, the present invention provides a method for detecting the arsenic content in quick-acting bezoar pills and its application. The detection method of the present invention can accurately detect the arsenic content in quick-acting bezoar pills, and has the advantages of high specificity, repeatability, stability and accuracy.

[0072] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A method for detecting the arsenic content in Suxiao Niuhuang Pills, characterized in that, It includes the following steps: (1) Mix quick-acting bezoar bolus, nitric acid and hydrochloric acid to obtain a mixed solution; digest the mixed solution to obtain a digested solution; add water to the digested solution to make the volume up to 50 mL to obtain a diluted solution; (2) Mix nitric acid, hydrochloric acid and water to obtain an acid solution; mix the acid solution and the diluted solution to obtain a sample solution; (3) Use atomic absorption spectrophotometry to measure the absorbance of the sample solution, and calculate the arsenic content in the quick-acting bezoar bolus according to the standard curve; The digestion process described in step (1) is as follows: heat the mixed solution from 30 °C to 120 °C, and keep it at 120 °C for 5 - 15 min; then heat it from 120 °C to 160 °C, and keep it at 160 °C for 10 - 20 min; then heat it from 160 °C to 180 °C, and keep it at 180 °C for 25 - 45 min; finally, cool it from 180 °C to 30 °C to obtain a digested solution.

2. The method according to claim 1, characterized in that The mass-to-volume ratio of the quick-acting bezoar bolus and nitric acid in step (1) is 0.05 - 0.3 g: 3 - 6 mL; The mass-to-volume ratio of the quick-acting bezoar bolus and hydrochloric acid is 0.05 - 0.3 g: 0.5 - 2 mL.

3. The method according to claim 2, wherein The digestion method described in step (1) is microwave digestion, and the digestion power is 750 - 1500 W.

4. The method according to claim 1, characterized in that The volume ratio of nitric acid, hydrochloric acid and water in step (2) is 3 - 6: 0.5 - 2: 42 - 46.5; The volume ratio of the acid solution and the diluted solution is 40 - 50: 4 - 7.

5. The method according to claim 1, characterized in that The wavelength of the measurement in step (3) is 193.7 nm.

6. The method according to claim 1, wherein The quick-acting bezoar bolus includes the following components in parts by mass: artificial bezoar 15 - 30 parts, concentrated water buffalo horn powder 40 - 60 parts, Coptis chinensis 20 - 40 parts, Scutellaria baicalensis 10 - 30 parts, Gardenia jasminoides 10 - 30 parts, borneol 3 - 10 parts, Curcuma aromatica 15 - 35 parts, cinnabar 10 - 35 parts, realgar 15 - 30 parts, Acorus tatarinowii 15 - 35 parts, mother-of-pearl 20 - 40 parts, refined honey 173 - 375 parts.

7. Use of the method according to any one of claims 1 - 6 in accurately detecting the arsenic content in quick-acting bezoar bolus.

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