时间:2024-07-28
Jiabao MA, Xiumei MA, Zhengteng YANG, Wen ZHONG, Chenglong WANG, Jiangcun WEI*
1.Guangxi International Zhuang Medicine Hospital, Nanning 530201, China; 2.The First Affiliated Hospital of Guangxi University of Chinese Medicine, Nanning 530023, China; 3.Guangxi Zhuang and Yao Pharmaceutical Engineering Technology Research Center, Nanning 530200, China
Abstract [Objectives]To establish a quality analysis method for Guangxi Zhuang medicine Lysimachia foenum-graecum Hance.[Methods]The moisture, total ash and alcohol-soluble extracts of L. foenum-graecum medicinal materials were determined in accordance with the inspection method of the Chinese Pharmacopoeia(2015).[Results]The 10 batches of L. foenum-graecum medicinal materials from different origins and different collection times in Guangxi all had the same plant morphology and medicinal properties.The moisture content was 5.69%-10.51%, the total ash content was 5.50%-8.61%, the acid-insoluble ash content was 0.42%-0.78%, and the extract was 15.28%-20.75%.[Conclusions]This study is expected to provide a scientific basis for the development and utilization of L. foenum-graecum medicinal materials and the establishment of its quality standards.
Key words Lysimachia foenum-graecum Hance, Character identification, Quality analysis
Guangxi Zhuang medicineLysimachiafoenum-graecumHance, also known as Linglingxiang, Xunxiang, Xiangcao, Peilan, and Paicao, is a plant of the genusLysimachiaL.of the Primulaceae family, mainly produced in Guangxi and Yunnan[1].It is a precious natural spice plant in Dayao Mountain of Guangxi.It is a precious Chinese herbal medicine.Its stem and leaves can be used as medicine.L.foenum-graecumhas the effects of invigorating the stomach, sweating, and relieving pain.It has remarkable effects on the treatment of colds, abdominal pain, eczema, cold and damp beriberi, traumatic abscess,etc., and has high medicinal value[2-3].In addition, it is a precious raw material for the spice industry.It forms the three major spices together withCinnamomumcassiaPresl,IlliciumverumHook.f.in Guangxi.It is widely used in the fragrance of high-end tobacco and wine[4].L.foenum-graecumhas pungent and sweet flavor and is warm in nature.It has the effects of clearing heat, promoting qi circulation, relieving pain, and repelling parasites.It is comply used to treat colds, headaches, sore throat, chest tightness and abdominal distension,etc.[4], so it has high medicinal value.The extracts and essential oils extracted fromL.foenum-graecumas raw materials have long-lasting and stable aromas and can be used to make tobacco and balsam[4-5].L.foenum-graecumis rich in a variety of active substances, such as flavonoids, triterpenoids, polyphenols and polysaccharides,etc.[6-7].
In order to develop Guangxi Zhuang medicineL.foenum-graecummedicinal resources and establish a scientific method for its quality control, we conducted systematic experimental research on the properties of Zhuang medicineL.foenum-graecummedicinal materials, various inspections of medicinal materials and determination of extracts.
2.1 Instruments101A-3E electric air blowing dryer(Shanghai Laboratory Instrument Works Co., Ltd.); SX2-4-10 box type resistance furnace-muffle furnace(Shanghai Laboratory Instrument Works Co., Ltd.); HWSZ6 electroheating thermostatic water bath(Shanghai Bluepard Instruments Co., Ltd.); pure water system(French Millipore Company); SQP electric balance(Sartorius Sartorius Scientific Instruments(Beijing)Co., Ltd.).
2.2 ReagentsEthanol(analytical reagent from Sinopharm Group Chemical Reagent Co., Ltd).
2.3 Medicinal materialsA total of 10 batches ofL.foenum-graecummedicinal materials used in the experiment were collected from different regions in Guangxi and dried at 55 ℃.They were identified by teacher from the Department of Pharmacy in the First Affiliated Hospital of Guangxi University of Chinese Medicine as the plant of the genusLysimachiaL.of the Primulaceae family,Lysimachiafoenum-graecumHance.The specific sources are listed in Table 1.
Table 1 Information of samples of Lysimachia foenum-graecum Hance
2.4 Moisture determinationWith reference to the moisture determination method specified in General Rule 0832 of 2015ChinesePharmacopoeiaVolume 4, we measured the moisture.Firstly, weighed 2.5 g ofL.foenum-graecumpowder and screened through No.2 sieve, placed these materials dried to constant weight in flat weighing bottle, the thickness less than 5 mm, loosened the test samples less than 10 mm, precisely weighed, opened the bottle cap and dried at 105 ℃ for 5 h, covered the cap, moved to a dry container, cooled for 30 min, and make precision measurement, dried at the 105 ℃ for one hour, cooled down and weighed, till the difference of two consecutive weighing not higher than 5 mg.Finally, calculated the moisture(%)of the medicinal material according to the loss of weight.
2.5 Measurement of ashes
2.5.1Determination of total ashes.With reference to the ash determination method specified in General Rule 2302 of 2015ChinesePharmacopoeiaVolume 4, took 4 g of medicinal powder, screened through No.2 sieve, placed in a crucible that was dried to constant weight, weighed(accurate to 0.01 g), and heated slowly, took care to avoid burning medicinal materials, and placed the crucible in the muffle furnace when it was completely carbonized.In the furnace, gradually increased the temperature to 600 ℃ to completely ash and reach the constant weight.Finally, calculated the total ashes(%)of the medicinal materials according to the residue weight.
2.5.2Determination of acid insoluble ash.Took the ash obtained above, slowly added about 10 mL of dilute hydrochloric acid to the crucible, covered the crucible with a watch glass, placed in a water bath and heated for 10 min, rinsed the watch glass with 5 mL of hot water, merged the washing liquid into the crucible, filtered with ash-free filter paper, washed the residue inside on filter paper with water, and washed until the lotion does not show chloride reaction.Moved the filter paper and filter residue to the same crucible, weighed, and heated it slowly.When it was completely carbonized, placed the crucible in the muffle furnace, and gradually increased the temperature to 600 ℃ to completely ash and reach the constant weight.Finally, calculated the acid insoluble ashes(%)of the medicinal materials according to the residue weight.
2.6 Determination of extractThe medicinal materials used for the determination need to be crushed to pass through the No.2 sieve and mix well.
2.6.1Selection of determination conditions.TookL.foenum-graecummedicinal materials produced in Jingxi City of Guangxi, used the pure water, 15% ethanol, 30% ethanol, 45% ethanol, 60% ethanol, 75% ethanol and 95% ethanol as solvents, determined the extract ofL.foenum-graecumin accordance with the extract determination method(cold soaking method and hot soaking method with the pure water and ethanol as solvent)specified in General Rule 2201 acid soluble extract determination of 2015ChinesePharmacopoeia(Volume 4).
2.6.2Determination method.The extract was determined in accordance with the extract measurement method specified in General Rule 2201 of 2015 Chinese Pharmacopoeia Volume 4.Precisely weighed 2.5 g of the medicinal material, placed in a 100-mL conical flask, accurately measured 60 mL of water, sealed the conical flask, weighed let it stand for one hour, and refluxed for one hour.After cooling down, removed the conical flask, sealed the conical flask, weighed, made up the weight using water, shook well, took 25 mL of filtrate, placed it in evaporating dish dried to constant weight, evaporated to dry state in water bath, dried for 3 h at 105 ℃, cooled for 30 min in a dry container, and rapidly and precisely weighed.Finally, calculated the extract(%)of Zhuang medicineL.foenum-graecummedicinal material according to the loss of weight.
3.1 Moisture determination resultsThe moisture of 10 batches of Zhuang medicineL.foenum-graecumfrom different origins and collection times in Guangxi was determined and the results are shown in Table 2.
Table 2 Determination results of moisture and extract content of Lysimachia foenum-graecum Hance(n=10, %)
From Table 2, it can be seen that there are certain differences in the moisture of 10 batches ofL.foenum-graecummedicinal materials in Guangxi and the average moisture content was 8.81%.The moisture content ofL.foenum-graecummedicinal materials collected in Fuchuan County, Guangxi in January, 2020 was the highest in the moisture determination of 10 batches ofL.foenum-graecummedicinal materials, which is 10.51%.Therefore, the limit was set at 120% of the highest value[8-11].Thus, it is tentatively determined that the moisture content of Guangxi Zhuang medicineL.foenum-graecumis not higher than 12.61%.
3.2 Ash content determination resultsThe ash content of 10 batches of Zhuang medicineL.foenum-graecumfrom different origins and collection times in Guangxi was determined and the results are shown in Table 3.
Table 3 Determination results of ash content of Lysimachia foenum-graecum Hance(n=10, %)
From Table 3, it can be seen that there are certain differences in the total ash and acid insoluble ash content of 10 batches ofL.foenum-graecummedicinal materials in Guangxi.The total ash content ofL.foenum-graecummedicinal materials collected in Bama County, Guangxi in December 2019 was the highest in 10 batches ofL.foenum-graecummedicinal materials, which is 8.61%.Therefore, the limit was set at 120% of the highest value[8-11].Thus, it is tentatively determined that the total ash content of Guangxi Zhuang medicineL.foenum-graecumis not higher than 10.33%.The acid insoluble ash content ofL.foenum-graecummedicinal materials collected in Tiane County of Hechi City, Guangxi in October 2019 was the highest in 10 batches ofL.foenum-graecummedicinal materials, which is 0.78%.Therefore, the limit was set at 120% of the highest value[8-11].Thus, it is tentatively determined that the acid insoluble ash content of Guangxi Zhuang medicineL.foenum-graecumis not higher than 0.94%.
3.3 Determination results of extractAccording to the experimental results, in the cold soaking method and hot soaking method, the extract content ofL.foenum-graecummeasured with 15% ethanol as the solvent was the highest, so 15% ethanol was used as the extraction solvent.
The 10 batches ofL.foenum-graecumfrom different origins and collection times in Guangxi were measured and the results are shown in Table 4.
There are certain differences in the extract content ofL.foenum-graecumin 10 batches ofL.foenum-graecummedicinal materials produced in Guangxi, the average extract content was 17.65%(Table 2).The extract content ofL.foenum-graecummedicinal materials collected in Binyang County, Guangxi in December 2019 was the highest in extract content determination of 10 batches ofL.foenum-graecummedicinal materials, which is 15.28%.Therefore, the limit was set at 80% of the lowest value[8-11].Thus, it is tentatively determined that the extract content of Guangxi Zhuang medicineL.foenum-graecumis not lower than 12.23%.
Table 4 Test by pure water, ethanol cold and hot soaking methods %
In this study, we determined the moisture content, ash and extract content of Zhuang medicineL.foenum-graecumfrom different origins and collection times in Guangxi.We obtained the following experimental results, the moisture content ofL.foenum-graecumwas not higher than 12.61%, total ash content was not higher than 10.33%, acid-insoluble ash content was not higher than 0.94%, and extract was not lower than 12.23%.The experimental results conform to the regulations, and the results show that different origins and collection times have an impact on the moisture, ash and extract content of the medicinal materials.Through this experiment, we carried out a preliminary study on the determination of the moisture content, ash, and alcohol soluble extract of theL.foenum-graecum.The experimental results are expected to provide a scientific basis for the development and use and establishing the quality control standard for Guangxi Zhuang medicineL.foenum-graecum.
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