Résumé
In this paper， the name， origin， producing area and other aspects of Menthae Haplocalycis Herba in the famous classical formulas were carried out by consulting herbal literature， medical books， prescription books in the past dynasties and related modern documents. Through the textual research， it can be seen that the name of Bohe was used as the correct name in the mainstream of the past dynasties， and there were still multiple synonyms， most of which originated from the false transmission of dialectal accent， producing area and efficacy. There are many varieties recorded in the literature of the past dynasties such as Bohe， Longnao Bohe， Hubohe and Shibohe. According to the textual research， Bohe， Longnao Bohe and Yebohe are consistent with Mentha haplocalyx， whcih is the mainstream variety. Longnao Bohe is named for its form of producing area， Shibohe is Mosla chinensis， Daye Bohe is Agastache rugosa， and Nanbohe is M. crispata. Menthae Haplocalycis Herba has been widely planted since Tang dynasty. It was mainly grown in Jiangsu， Zhejiang， Jiangxi and Sichuan in Ming and Qing dynasties， and Jiangsu is the genuine production area. Its quality is best if it has dry body， no roots， many leaves， green color and strong smell. In ancient times， the stems and leaves of Menthae Haplocalycis Herba were often picked and dried in summer and autumn， which is basically the same as the records of modern times when the stems and leaves are luxuriant in summer and autumn， or when the flowers bloom to three rounds， they are picked in sunny days and cut in different times， and then dried in the sun or in the shade， and the raw products was often used as medicine in ancient and modern times. Before the Song dynasty， Menthae Haplocalycis Herba was recorded as pungent and warm. Until the Song dynasty， it was written as “extremely cool” in Lyuchanyan Bencao. It may have been thought in the early stage that it was similar to several warm herbs， such as Perilla frutescens， Stachys japonica， Elsholtzia ciliata and M. chinensis in appearance， all of which have the function of Xinsan， so it was recorded as warm. Since the Qing dynasty， Menthae Haplocalycis Herba has been recorded as cool property in the mainstream materia medica， Menthae Haplocalycis Herba recorded as pungent and cool in the 2020 edition of Chinese Pharmacopoeia， and its effect is to dissipate wind heat， clear the head， relieve the pharynx and so on， the records of efficacy in ancient and modern times are basically the same. Based on the research results， it is suggested that raw products of M. haplocalyx should be selected when developing the famous classical formulas containing Menthae Haplocalycis Herba.
Résumé
Considering the characteristic chromatograms and quality value transmitting of three volatile components, this study investigated the changes in volatile components of Menthae Haplocalycis Herba in each heating process of personalized preparations and identified the critical control points for the application of volatile components from traditional Chinese medicine in such preparations. The characteristic chromatograms of volatile components in Menthae Haplocalycis Herba were established by gas chromatography, followed by the quantitative determination of three volatile components menthone, menthol, and piperitone and the comparison of retention rates of volatile components during the crushing, extraction, concentration and drying of preparation products and their change rules in characteristic peaks. The results showed that the volatile components of Menthae Haplocalycis Herba were reduced in each process. The loss rate was low in the crushing process when the volatile component peaks were present, but high in the extraction and concentration processes, manifested as the absence of partial component peaks and the presence of new component peaks. The changes in volatile components of Chuanxiong Chatiao Granule in the drying process were compared with those in Chuanxiong Chatiao Pill, both of which were prepared from the raw Menthae Haplocalycis Herba powder, and the findings demonstrated that Chuanxiong Chatiao Pill was superior to Chuanxiong Chatiao Granule. This study confirmed that the retention rates of volatile components in Menthae Haplocalycis Herba were mostly affected by the extraction and concentration processes, and the packing of preparations helped to reduce the loss of volatile components in Menthae Haplocalycis Herba powder, which has provided reference for the application of Chinese medicinal materials containing volatile components in the personalized preparations.
Sujets)
Médicaments issus de plantes chinoises , Médecine traditionnelle chinoise , PoudresRésumé
To establish the method for determining non-volatile ingredients of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, isochlorogenic acid A, rosmarinic acid, ferulic acid, rutin, luteoloside, isoquercitrin, hesperidin, diosmin, diosmetin, luteolin, acacetin and linarin in Menthae Haplocalycis Herba formula granules and traditional herbal pieces by UPLC-MS/MS, and analyze the correlation of non-volatile ingredients in Menthae Haplocalycis Herba formula granules and traditional herbal pieces. Shim-pack GIST C_(18) column(2.1 mm×100 mm, 2 μm) was adopted with acetonitrile-0.1% formic acid aqueous solution as the mobile phase for gradient elution at the flow rate of 0.4 mL·min~(-1). The column temperature was set at 35 ℃. The quantitative analysis was performed using the electrospray ionization source and the multiple reaction monitoring. The linear relationship, resolution, repeatability and recovery of the 16 chemical components all met the requirements. The 16 non-volatile ingredients in traditional herbal pieces of Menthae Haplocalycis Herba could be tracked in formula granules. There were certain differences of the 16 chemical components among Menthae Haplocalycis Herba formula granules of different manufacturers and traditional herbal pieces of different producing areas. The UPLC-MS/MS method was simple, rapid and accurate, and could be used for the quality control of non-volatile ingredients in Menthae Haplocalycis Herba formula granules and traditional herbal pieces.
Sujets)
Chromatographie en phase liquide à haute performance , Chromatographie en phase liquide , Corrélation de données , Médicaments issus de plantes chinoises , Spectrométrie de masse en tandemRésumé
Objective:To research optimum compatibility components ratio for the anti-influenza virus effect of different compatibility of Menthae Haplocalycis Herba-Schizonepetae Herba. Method:The 228 SPF grade ICR rats of half male and half female were randomly divided into 19 groups, with 12 rats in each group. In each group, the ratio of flavonoids and volatile oil was determined. ICR rats were anesthetized with ether and infected with influenza A virus A/PR/8/34 (H1N1) with A 10-fold lethal dose（LD50）50 μL nasal drip infection. Than the blank control group was treated with the same amount of normal saline nasal drip control, and the rats were given the drug by gavage on the day after virus infection, the blank group and model group were given the same amount of distilled water, and the positive control group were given Oseltamivirphosphate and compound Jinyinhua granules by gavage, and once a day for 7 days. Different compatibility of volatile oil and flavonoids in Menthae Haplocalycis Herba and Schizonepetae Herba are applied to rats infected with influenza A/PR8/34 (H1N1) virus to study the pharmacodynamic screening by lung index of influenza-infected mice and histopathological examination. And antiviral effects as well as the expression of interleukin-6（IL-6）, interleukin-1β（IL-1β）, tumor necrosis factor-α (TNF-α) is studied. Result:Lung infection injury was prepared by infecting mice with influenza A virus A/ pr8/34(H1N1). Lung mass increased at the end of the experiment in the model group, and lung index was compared with that in the blank group(P<0.01). And the experimental lung weight of oseltamivirphosphate group, compound Jinyinhua granules group, volatile oil 1-volatile oil 2 group, volatile oil 1 group and volatile oil 2 group were compared with that of the model group (P<0.05). Lung index of Oseltamivirphosphate group and volatile oil group was compared with that of model group (P<0.01).Lung index of compound Jinyinhua granules group, volatile oil 1-volatile oil 2 group, volatile oil 2-flavonoids 2 group, volatile oil 1-volatile oil 2-flavonoids 1 group, volatile oil 1-volatile oil 2-flavonoids 2 group, volatile oil 1-volatile oil 2-flavonoids 2 group, volatile oil 1-volatile oil 2-flavonoids 2 group and volatile oil 2 group were compared with the model group (P<0.05). And antiviral effect as well as the expression of IL-6, IL-1β, TNF-α is studied. The expression levels of IL-6, IL-1β, TNF-α in volatile oil 1-flavonoids 1 group, volatile oil 1-flavonoids 2 group, volatile oil 1-volatile oil 2 group, volatile oil 1-volatile oil 2-flavonoids 1 group, volatile oil 1-volatile oil 2-flavonoids 2 group, volatile oil 2 groups, flavonoids 2 groups were decreased, compared with the model group (P<0.01). Conclusion:It is found that different combinations have better biological effects and good antiviral effects. This study explores the synergies compatibility rule and mechanism of action on Menthae Haplocalycis Herba and Schizonepetae Herba pairs, which will not only develop the theory of Chinese medicine compatibility but also contribute to laying a foundation for the innovation of the influenza virus drug development.
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Objective: To establish an HPLC fingerprint of Menthae Haplocalycis Herba standard decoction,in order to identify the main chemical component of common peaks,and determine the content of rosmarinic acid. Method: The chromatographic fingerprints of 10 batches of Menthae Haplocalycis Herba standard decoction from different areas were determined,and the chromatographic separation was carried out on Kromasil C18 (4.6 mm×250 mm,5 μm) at the temperature of 30℃. The mobile phase was acetonitrile and 0.1%formic acid solution for gradient elution,with a flow rate of 1 mL·min-1,and the detection wavelength was 330 nm. The 10 batches of fingerprints were imported into Similarity Evaluation System for Chromatographic Fingerprint of TCM (2012.130723) for chromatographic peak matching, the reference fingerprint was established with the average method,and the similarities of 10 batches were evaluated. Result: The HPLC fingerprint of Menthae Haplocalycis Herba showed 13 common peaks. The similarities of 10 batches from different areas were all more than 0.90.At the same time,9 common peaks of the fingerprint were identified by using Q-TOF-MS spectrometry. Rosmarinic acid content was also determined by using the HPLC fingerprint method. Conclusion: The method is simple,rapid and accurate,with a good reproducibility, and can be used to rapidly and effectively evaluate the quality of Menthae Haplocalycis Herba standard decoction and lay a foundation for the quality control of Menthae Haplocalycis Herba formula granules.
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Objective To compare the chemical composition and antibacterial activity of the volatile oils from Forsythiae Fructus (FF), Schizonepetae Herba (SH), Menthae Haplocalycis Herba (MH), and their compatibility, and to explore the influence of different extraction methods on components and antibacterial activity of volatile oil. Methods GC-MS was employed to analyze the composition of the volatile oil from FF, SH, and MH extracted separately, and their mixture extracted, as well as physical mixing volatile oil of FF, SH, and MH extracted separately. The diameter of the inhibition zone and the minimum inhibitory concentration (MIC) were measured using the paper agar diffusion method and micro dilution method. The antibacterial activities of volatile oil on four common pathogens of respiratory tract were evaluated. Results When FF, SH, and MH were mixed and extracted, the main obtained components and contents of volatile oil changed. Compared to separately extracted volatile oil, eight new components emerged, seven components from FF and seven components from SH disappeared in FF and SH mixture extracted volatile oil. In FF and MH mixture extracted volatile oil, compared with separately extracted, six components from FF and eight components from MH disappeared, and eight new components emerged. As to SH and MH mixture extracted volatile oil, four components from SH and seven components from MH disappeared, and seven new components emerged. In the three herbs mixture extracted volatile oil, six components from FF, four components from SH, and two components from MH disappeared, one commom component of FF and MH, two common components of SH and MH disappeared, however, nine new components emerged. The content of pulegone significantly decreased in the three herbs mixture extracted volatile oil compared with that in separately extracted. The antibacterial experiments showed that the antibacterial effects of the volatile oils obtained by different extraction methods were different. The antibacterial effects of volatile oil extracted separately and their physical mixing volatile oil on Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, and Candida albicans were better than that from mixture extracted. Conclusion Volatile oil is an important effective component of Chinese patent medicines with relieving exterior syndrome function. Different extraction methods have a certain influence on the yield and composition of volatile oil, which ultimately affects the efficacy of drugs. Therefore, we should pay more attention to extraction method and process of volatile oil in these prescriptions.
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Objective: To establish a method for the determination of three main volatile components (menthone, menthol, and pulegone) in Yinqiao Powder (YQP) distillate and provide the evidence for elucidating the scientific connotation of its traditional decocting method "taking when the fragrance volatilized fiercely". Methods: YQP distillates with different decocting time were prepared to study the dynamic changes of chemical components during decocting process. GC-MS was used to analyze the volatile components qualitatively and determine the contents of menthone, menthol, and pulegone in YQP distillate. Results: GC-MS total ion chromatograms of YQP volatile oil included 26 peaks, of which the relative contents of 14 peaks were greater than 1.5%, mainly from Forsythiae Fructus, Menthae Haplocalycis Herba, and Schizonepetae Herba. With the extension of the boiling time, the evaporation rates of menthone, menthol, and pulegone all increased to maximum and then decreased gradually. When boiling for 5-10 min, the maximum average evaporation rates of menthone, menthol, and pulegone were 13.77, 147.74, and 31.26 ìg/min, respectively. When boiling for 0-5, 5-10, 10-15, 15-20, 20-25, 25-30, 30-40, 40-50, 50-60, 60-80, 80-100, and 100-120 min, the average evaporation rates of total three volatile components were 160.23, 192.77, 120.71, 70.85, 54.01, 42.41, 30.36, 17.87, 14.98, 10.01, 7.79, and 7.58 ìg/min, respectively. Conclusion: The evaporation rates of menthone, menthol, and pulegone in YQP are heavily influenced by decocting time. The fragrance is volatilized fiercely at about 5 min after boiling, while the average evaporation rates of menthone, menthol, and pulegone are high, so after boiling for 5-10 min, menthone, menthol, and pulegone were evaporated a lot. The fragrance gets weak after 15 min of boiling, the average evaporation rates of menthone, menthol, and pulegone are decreasing heavily. It is suggested that the traditional decocting method has some scientific foundation.
Résumé
Menthae Haplocalycis Herba has been widely applied in such fields as food, cosmetics, daily necessities, medicine and health, due to its unique efficacy. However, as the safety of traditional Chinese medicines has been of increasing concern, the quality issue of Menthae Haplocalycis Herba and its decoction slices has become a key obstructive factor for exports. This article focused on the control over Menthae Haplocalycis Herba's adulterants, exogenous hazardous residues and internal properties (chemical compositions, spectrum effect relationship). Moreover, current studies on the quality of Menthae Haplocalycis Herba and its decoction slices, as well as the existing problems in recent years were systematically summarized in the expectation of improving the means of quality control of Menthae Haplocalycis Herba and its decoction slices, enhancing its quality standards, and ensuring the use safety and effectiveness.