Abstract Atomic absorption spectrometry was used to determine Ca, Mg and Fe in 7 traditional Chinese medicines including Gengchuan Tablet, Fufang Banxia Tablet, Weitongning Tablet, Boxing Tablet, Shenqi Jiangtang Capsule, Xia Sangju Granule and American Ginseng Tablet. , Zn, K, Na, Mn, Cu, Cr, Co, Sr, Ni, Cd and Pb elements. The effects of the type of digestive juice (mixed acid), the ratio of HNO3 and HClO4 in the mixed acid, the volume of the digestive juice and the digestion time on the determination results were studied in detail. The results showed that the contents of Ca, Mg, Fe, K and Na were generally rich in the selected seven drugs. The Mn content in the Shenqi Jiangtang Capsules for the treatment of diabetes was rich, while the Suppressant Tablets were rich in Sr. , Mn and Cu elements.
Key words: atomic absorption spectrometry; proprietary Chinese medicine; trace elements In recent years, trace elements have attracted people's interest in the study of inorganic elements, especially trace elements in proprietary Chinese medicines, due to their enormous biological functions, physiological functions and practical value of clinical diagnosis and treatment. . Modern research shows that in the process of exerting the efficacy of Chinese patent medicines, the synergistic effect of trace elements can not be ignored. The proper amount of trace elements can not only promote the growth and development of the body, but also improve the immune function of the body and reduce the susceptibility of humans to diseases. The determination of trace elements can provide basic data for clarifying the mechanism of action, modification and innovation of new drugs, and can also provide basis for the identification and improvement of Chinese medicinal materials. Atomic absorption spectroscopy has the advantages of high sensitivity, good selectivity, high precision and fast analysis speed. In this paper, the atomic absorption spectrometry was used to determine the Ca, Mg in the traditional Chinese medicines such as Gengchuan Tablet, Fufang Banxia Tablet, Weitongning Tablet, Boxing Tablet, Shenqi Jiangtang Capsule, Xia Sangju Granule and American ginseng Tablet. The content of Fe, Zn, K, Na, Mn, Cu, Cr, Co, Sr, Ni, Cd and Pb. The effects of the type of digestive juice (mixed acid), the ratio of HNO3 and HClO4 in the mixed acid solution, the volume of the digestive juice and the digestion time on the measurement results were studied in detail. This study can provide some information for analyzing the relationship between the efficacy of the above-mentioned proprietary Chinese medicines and trace elements, clarifying its mechanism of action, and transforming and innovating new drugs.
1 Experimental part
1.1 Instrument and working conditions
WFX-1F2B2 atomic absorption spectrophotometer (Beijing Second Optical Instrument Factory, with microcomputer and printer), 14 element hollow cathode lamps.
1.2 reagents and standard solutions
Standard solutions of 14 elements (Ca, Mg, Fe, Zn, K, Na, Mn, Cu, Cr, Co, Sr, Ni, Cd, Pb) were purchased from the National Standards Research Center (concentration of stock solution except Cr The remaining elements were 100 μg/mL except for 1 000 μg/mL. HNO3 (A1R1, Xinyang Chemical Reagent Factory), HClO4 (A1R1, Shanghai Taopu Chemical Plant), H2SO4 (A1R1, Beijing Chemical Reagent Factory), HCl (A1R1, Xinyang Chemical Reagent Factory), H2O2 (A1R1, Shanghai Taopu Chemical Plant) ). The experimental water is ultrapure water (UPW225N, Beijing General Instrument Company).
1.3 Sample source and treatment The 7 kinds of Chinese patent medicines used in the experiment: Guchuanchuan Tablet, Compound Banxia Tablet, Weitongning Tablet, Boxing Tablet, Shenqi Jiangtang Capsule, Xia Sangju Granule, American American Ginseng Tablet are all commercially available.
Preparation of the sample solution: Take an appropriate amount of the drug (the pellet is preliminarily ground with a mortar, and the capsule is filled with the inner capsule), placed in an electric drying oven, dried at 100 ° C for 1 h, cooled and placed in a desiccator. Accurately weigh about 1g of drug in a 100mL small beaker, add 20mL HNO3-HClO4 (3:1) mixed acid, heat digestion for 40 min, quantitative transfer and make up to 100mL. Take the supernatant for measurement (if necessary, appropriate dilution).
2 Results and discussion
2.1 Optimization of sample processing conditions
2.1.1 Selection of mixed acid species In order to find a suitable digestive system, the effects of several digestion systems of HNO3-HClO4, HNO3-HCl, HNO3-H2SO4 and HNO3-H2O2 on the determination results were studied. The experimental results show that it is suitable to use HNO3-HClO4 mixed acid system as digestive solution.
2.1.2
The effect of HNO3 and HClO4 volume ratio in HNO3-HClO4 mixed acid was determined by taking the content of Cu, Fe, Zn, Mn and Ni in the ginseng tablets as an example. The volume ratio of HNO3 and HClO4 in the mixed acid digest was 1:1, 3 : 1 , 4:1 , 5:1 , 7:1 , 9:1 effect. Visible, HNO3
When the volume ratio of -HClO4 is 3:1, the digestion effect is good.
2.1.3 The influence of digestion time is still determined by the determination of Cu, Fe, Zn, Mn and Ni. The mixed acid of HNO3-HClO4 with a volume ratio of 3:1 is used as the digestion system, and the volume of fixed mixed acid is 15mL. The digestion time is studied. The effect on the measurement results. The results showed that the digestion time of 40 minutes can achieve the good digestive effect of Zui.
2.1.4 Influence of digestive juice volume The 3:1 HNO3-HClO4 mixed acid system was used as the digestive juice with a fixed digestion time of 40 min and a sample mass of 1.0 g. The volume of mixed acid was 8 , 12 , 16 , 20 , respectively . The effect on the measurement results at 24 mL (still taking the determination of Cu, Fe, Zn, Mn and Ni in the boxing tablets as an example). It can be seen that the mixed acid volume is 20 mL to obtain satisfactory measurement results.
2.2 Standard curve and method Accuracy test The stock solution of 14 elements is diluted into a series of standard solutions with appropriate concentration. The standard calibration curve method is used to determine the instrument conditions listed in Table 1. The results show that the working curves of the 14 elements are all straight lines, and the correlation coefficients are all greater than 0.997, indicating that the linear relationship of the working curve is good. In order to further investigate the accuracy of the method, the spiked recovery test was carried out by taking the boxing ginseng as an example (to ensure the accuracy, the standard addition recovery test was done in parallel, each parallel determination was 3 times, and then the average value was taken).
2.3 Sensitivity and detection limits The sensitivity and detection limits of the method were calculated according to the literature.
2.4 Determination of 14 trace elements in the sample Accurately weigh 1.0 g of sample and treat the sample according to the sample processing method in Section 1.3. The sample solution was measured according to the working conditions of the instruments listed in the table. Place
2.5 Discussion From the measurement results, it can be seen that the content of five elements of Ca, Mg, Fe, K and Na in the selected seven Chinese patent medicines is generally rich. However, with the different effects of variety and function, the content of trace elements in each drug is also very different. It is also not accidental if the Mn content is higher in the treatment of diabetes drugs. Animal experiments have shown that when the body is deficient in Mn, its insulin B cells decrease, pancreatic hypoplasia, glucose tolerance decreases, and glucose utilization rate decreases accordingly. Stomach pain tablets contain high levels of Sr, Mn and Cu. At the same time, harmful Cd and Pb are also present in certain drugs. These harmful elements may come from raw materials, solvents or some parts of the processing process, and should be of concern.
references
[1] DONG Shun2fu, ZHU Zhi2guo (Dong Shunfu, Zhu Zhiguo) . Spectroscopy and Spectral Analysis , 2002 , 22 (3) : 478.
[ 2 ] FU Ke2jun (Foke Army) . Trace Elments in Human Body . Beijing : Chinese Medicine Science and Technology Press (Beijing: China Medical Science and Technology Press), 1995. 82.
Key words: atomic absorption spectrometry; proprietary Chinese medicine; trace elements In recent years, trace elements have attracted people's interest in the study of inorganic elements, especially trace elements in proprietary Chinese medicines, due to their enormous biological functions, physiological functions and practical value of clinical diagnosis and treatment. . Modern research shows that in the process of exerting the efficacy of Chinese patent medicines, the synergistic effect of trace elements can not be ignored. The proper amount of trace elements can not only promote the growth and development of the body, but also improve the immune function of the body and reduce the susceptibility of humans to diseases. The determination of trace elements can provide basic data for clarifying the mechanism of action, modification and innovation of new drugs, and can also provide basis for the identification and improvement of Chinese medicinal materials. Atomic absorption spectroscopy has the advantages of high sensitivity, good selectivity, high precision and fast analysis speed. In this paper, the atomic absorption spectrometry was used to determine the Ca, Mg in the traditional Chinese medicines such as Gengchuan Tablet, Fufang Banxia Tablet, Weitongning Tablet, Boxing Tablet, Shenqi Jiangtang Capsule, Xia Sangju Granule and American ginseng Tablet. The content of Fe, Zn, K, Na, Mn, Cu, Cr, Co, Sr, Ni, Cd and Pb. The effects of the type of digestive juice (mixed acid), the ratio of HNO3 and HClO4 in the mixed acid solution, the volume of the digestive juice and the digestion time on the measurement results were studied in detail. This study can provide some information for analyzing the relationship between the efficacy of the above-mentioned proprietary Chinese medicines and trace elements, clarifying its mechanism of action, and transforming and innovating new drugs.
1 Experimental part
1.1 Instrument and working conditions
WFX-1F2B2 atomic absorption spectrophotometer (Beijing Second Optical Instrument Factory, with microcomputer and printer), 14 element hollow cathode lamps.
1.2 reagents and standard solutions
Standard solutions of 14 elements (Ca, Mg, Fe, Zn, K, Na, Mn, Cu, Cr, Co, Sr, Ni, Cd, Pb) were purchased from the National Standards Research Center (concentration of stock solution except Cr The remaining elements were 100 μg/mL except for 1 000 μg/mL. HNO3 (A1R1, Xinyang Chemical Reagent Factory), HClO4 (A1R1, Shanghai Taopu Chemical Plant), H2SO4 (A1R1, Beijing Chemical Reagent Factory), HCl (A1R1, Xinyang Chemical Reagent Factory), H2O2 (A1R1, Shanghai Taopu Chemical Plant) ). The experimental water is ultrapure water (UPW225N, Beijing General Instrument Company).
1.3 Sample source and treatment The 7 kinds of Chinese patent medicines used in the experiment: Guchuanchuan Tablet, Compound Banxia Tablet, Weitongning Tablet, Boxing Tablet, Shenqi Jiangtang Capsule, Xia Sangju Granule, American American Ginseng Tablet are all commercially available.
Preparation of the sample solution: Take an appropriate amount of the drug (the pellet is preliminarily ground with a mortar, and the capsule is filled with the inner capsule), placed in an electric drying oven, dried at 100 ° C for 1 h, cooled and placed in a desiccator. Accurately weigh about 1g of drug in a 100mL small beaker, add 20mL HNO3-HClO4 (3:1) mixed acid, heat digestion for 40 min, quantitative transfer and make up to 100mL. Take the supernatant for measurement (if necessary, appropriate dilution).
2 Results and discussion
2.1 Optimization of sample processing conditions
2.1.1 Selection of mixed acid species In order to find a suitable digestive system, the effects of several digestion systems of HNO3-HClO4, HNO3-HCl, HNO3-H2SO4 and HNO3-H2O2 on the determination results were studied. The experimental results show that it is suitable to use HNO3-HClO4 mixed acid system as digestive solution.
2.1.2
The effect of HNO3 and HClO4 volume ratio in HNO3-HClO4 mixed acid was determined by taking the content of Cu, Fe, Zn, Mn and Ni in the ginseng tablets as an example. The volume ratio of HNO3 and HClO4 in the mixed acid digest was 1:1, 3 : 1 , 4:1 , 5:1 , 7:1 , 9:1 effect. Visible, HNO3
When the volume ratio of -HClO4 is 3:1, the digestion effect is good.
2.1.3 The influence of digestion time is still determined by the determination of Cu, Fe, Zn, Mn and Ni. The mixed acid of HNO3-HClO4 with a volume ratio of 3:1 is used as the digestion system, and the volume of fixed mixed acid is 15mL. The digestion time is studied. The effect on the measurement results. The results showed that the digestion time of 40 minutes can achieve the good digestive effect of Zui.
2.1.4 Influence of digestive juice volume The 3:1 HNO3-HClO4 mixed acid system was used as the digestive juice with a fixed digestion time of 40 min and a sample mass of 1.0 g. The volume of mixed acid was 8 , 12 , 16 , 20 , respectively . The effect on the measurement results at 24 mL (still taking the determination of Cu, Fe, Zn, Mn and Ni in the boxing tablets as an example). It can be seen that the mixed acid volume is 20 mL to obtain satisfactory measurement results.
2.2 Standard curve and method Accuracy test The stock solution of 14 elements is diluted into a series of standard solutions with appropriate concentration. The standard calibration curve method is used to determine the instrument conditions listed in Table 1. The results show that the working curves of the 14 elements are all straight lines, and the correlation coefficients are all greater than 0.997, indicating that the linear relationship of the working curve is good. In order to further investigate the accuracy of the method, the spiked recovery test was carried out by taking the boxing ginseng as an example (to ensure the accuracy, the standard addition recovery test was done in parallel, each parallel determination was 3 times, and then the average value was taken).
2.3 Sensitivity and detection limits The sensitivity and detection limits of the method were calculated according to the literature.
2.4 Determination of 14 trace elements in the sample Accurately weigh 1.0 g of sample and treat the sample according to the sample processing method in Section 1.3. The sample solution was measured according to the working conditions of the instruments listed in the table. Place
2.5 Discussion From the measurement results, it can be seen that the content of five elements of Ca, Mg, Fe, K and Na in the selected seven Chinese patent medicines is generally rich. However, with the different effects of variety and function, the content of trace elements in each drug is also very different. It is also not accidental if the Mn content is higher in the treatment of diabetes drugs. Animal experiments have shown that when the body is deficient in Mn, its insulin B cells decrease, pancreatic hypoplasia, glucose tolerance decreases, and glucose utilization rate decreases accordingly. Stomach pain tablets contain high levels of Sr, Mn and Cu. At the same time, harmful Cd and Pb are also present in certain drugs. These harmful elements may come from raw materials, solvents or some parts of the processing process, and should be of concern.
references
[1] DONG Shun2fu, ZHU Zhi2guo (Dong Shunfu, Zhu Zhiguo) . Spectroscopy and Spectral Analysis , 2002 , 22 (3) : 478.
[ 2 ] FU Ke2jun (Foke Army) . Trace Elments in Human Body . Beijing : Chinese Medicine Science and Technology Press (Beijing: China Medical Science and Technology Press), 1995. 82.
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