Quality Control Of Medicinal Plants Research Articles

Separation, identification, and fingerprinting of antioxidant components in persimmon (Diospyros kaki) leaves by offline two-dimensional liquid chromatography with electrochemical detection and tandem mass spectrometry.

In this work, the antioxidant components in persimmon (Diospyros kaki) leaves were separated by offline two-dimensional liquid chromatography-electrochemical detection (LC×LC-ECD) and identified by LC-tandem mass spectrometry (LC-MS/MS). A total of 33 antioxidants, mainly proanthocyanidins, and glycosides of kaempferol and quercetin, were identified. The antioxidant assays demonstrated that the fractions collected from the first-dimension LC (1D-LC) possessed considerable radical scavenging capabilities, with correlation coefficients of peak area versus radical scavenging capability of 1,1-diphenyl-2-picrylhydrazyl and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) being 0.9335 and 0.9116, respectively. The fingerprinting showed that 37 peaks were present in all samples. The major antioxidant components of persimmon leaves were the glycosides of kaempferol and quercetin. Finally, fourteen antioxidants were quantitatively assessed. Offline LC×LC provided high peak capacity and separation; ECD enabled specific screening and detection of antioxidant components; and MS/MS provided excellent identification capability. In this study, the combination of the three approaches was utilized to screen for antioxidant components in persimmon leaves, with satisfactory findings. In conclusion, this technique is an effective means for rapid analysis of antioxidant components and quality control of medicinal plants, achieving rapid separation of congeners and facilitating more accurate qualitative and quantitative analyses.

Determination of pesticide residues and heavy metals in Adhatoda Vasaka Linn.

Heavy metals and pesticide residue analysis plays an important role in the quality control of medicinal plants like Vasaka (Adhatoda vasica). Hence a study was conducted to determine heavy metals and pesticide residues in this medicinal herb, which is a highly useful commodity in the health system. The reliable, rapid and nontoxic sample preparation method like QuEChERS and analytical methods like GC-MS were proposed for the simultaneous determination of pesticide residues and Heavy metal detection was carried out by ICP-MS. In this study, the presence of organophosphorus and organochlorine pesticides like alachlor, heptachlor, heptachlor epoxide, aldrin, dieldrin, endrin, etc was checked but not detected. Heavy metals like Arsenic (As), Cadmium (Cd), Mercury (Hg) and Lead (Pb) are traced in samples about 2.3005 ppb, 0.799 ppb, 2.290 ppb and 10.204 ppb respectively in the present study.

Quality parameters for the medicinal plant Drosera rotundifolia L.: A new approach with established techniques.

Monographs of the European Pharmacopoeia (Ph. Eur.) are the basis for quality control of medicinal plants and therefore important to ensure the consistency, quality, safety, and efficacy of phytopharmaceuticals. The traditional medicinal plant sundew (Drosera sp.) has disappeared from therapy due to nature conservation, but can now be cultivated sustainably on rewetted peatland. However, currently there is no valid Ph. Eur. monograph for the quality control of Droserae herba. In this study, sundew material from different species and sources was investigated with the aim of developing quality control methods based on the Ph. Eur. and defining a uniform quality standard for Droserae herba. It was possible to distinguish between sundew species of different quality, using macroscopic, microscopic, and chromatographic methods. Special emphasis was laid on the content of flavonoids and naphthoquinones as important quality parameters as their content differed between the sundew species. The differences in content and toxicity result in the recommendation that only round-leaved sundew (Drosera rotundifolia L.) should be used as a medicinal plant for the production of phytopharmaceuticals in the future.

Determination of Total Sennosides and Sennosides A, B, and A1 in Senna Leaflets, Pods, and Tablets by Two-Dimensional qNMR

In the present work, a two-dimensional qNMR method for the determination of sennosides was established. Using band-selective HSQC and the cross correlations of the characteristic 10-10' bonds, we quantified the total amount of the value-determining dianthranoids in five minutes, thus, rendering the method not only fast, but also specific and stability indicating. The validation of the method revealed excellent accuracy (recovery rates of 98.5 to 103%), precision (RSD values of 3.1%), and repeatability (2.2%) and demonstrated the potential of 2D qNMR in the quality control of medicinal plants. In a second method, the use of 2D qNMR for the single analysis of sennosides A, B, and A1 was evaluated with acceptable measurement times (31 min), accuracy (93.8%), and repeatability (5.4% and 5.6%) for the two major purgatives sennoside A and B. However, the precision for sennoside B and A1 was not satisfactory, mainly due to the low resolution of the HSQC signals of the two compounds.

Green chromatography as a novel alternative for the quality control of Serjania marginata Casar. Leaves

In the quest for efficient sustainable alternative techniques for the quality control of medicinal plants, the present work sought to develop a green chromatographic method for the fingerprinting and standardization of the extract of Serjania marginata leaf – plant species used in folk medicine for the treatment of stomach ache. The analytical method was developed using the HPLC-PDA technique with only ethanol and water as solvents and based on the application of fractional factorial planning for the screening of variables and Doehlert matrix for the optimization procedure. The proposed green chromatographic method was compared with the HPLC method reported in the literature using the following metrics and taking into account the chromatographic performance and environmental impact of the methods: Green Chromatographic Fingerprinting Response (GCFR), HPLC-EAT (EAT – Environmental Assessment Tool), Analytical GREEnness (AGREE) and Green Analytical Procedure Index (GAPI). The green chromatographic technique was validated through the analysis of the following parameters: selectivity, linearity, detection and quantification limits, precision and robustness, while the standardization of the extract was performed through the quantification of protocatechuic acid, (+)-catechin, (–)-epicatechin, and apigenin derivatives. The optimum conditions for the application of the proposed chromatographic method were as follows: linear gradient from 10 to 55% of ethanol in 35 min, temperature of 60 °C, flow rate of 1.11 mL min−1, and phenyl hexyl column. Under these conditions, a desirability value of 0.93866 was obtained with maximum responses of 25.327 and 12.189, for peak number and GCFR, respectively. In addition, the analysis of the plant extract by HPLC-MS/MS, under the same optimized method, allowed the annotation of 21 phenolic compounds, including a phenolic acid, proanthocyanidins and flavonoids derived from quercetin, apigenin and luteolin. The results obtained show that the proposed method has good accuracy and robustness, apart from being environmentally friendly – once it satisfies the principles of Green Chemistry.

Improving the Extraction of Active Ingredients from Medicinal Plants by XynA Modification

Active ingredients of medicinal plants have unique pharmacological and clinical effects. However, conventional extraction technology has many disadvantages, such as long-time and low-efficiency. XynA-assisted extraction may overcome such problems, since the plant cell wall is mainly composed of cellulose. Based on the three-dimensional protein structure, we found the C-terminal domain and N-terminal domain twisted together and resulted in more flexibility. We carried out a series of truncations, with XynA_ΔN36 getting more yields of active ingredients. As shown by HPLC analysis, the efficiencies for extraction of salvianic acid A and berberine from Salvia miltiorrhiza and Phellodendron chinense were increased by approximately 38.14% and 35.20%, respectively, compared with the conventional extraction protocol. The yields of the two compounds reached 2.84 ± 0.05 mg g−1 and 3.52 ± 0.14 mg g−1, respectively. Above all, XynA_ΔN36 can be applied to the extraction of salvianic acid A and berberine, and this study provides a novel enzyme for the extraction technology, which aids rational utilization and quality control of medicinal plants.

Heavy Metal Content Screening in Leaves and Flowers of Hypericum montbretii Spach. by Atomic Absorption Spectrometry

Atomic absorption spectrometry facilitates the reliable determination of mineral content during pharmaceutical quality control of medicinal plants. In the present work, measurable amounts of Fe, Ca, Cu, K, Mg, Mn, Na and Zn were detected in the leaves and flowers of Hypericum montbretii Spach. through atomic absorption spectrometry. Mean heavy metal content in the flowers and leaves of H. montbretii Spach. was, in descending order, Ca > Mg > K > Mn> Na. Ca was present in higher concentrations in the leaves (10252.75 ppm) and flowers (7321.94 ppm) of titled plant. Our results reveal that flowers are less suitable as target plant parts for metal accumulation than leaves.

Heavy Metal Content Screening in Leaves and Flowers of Hypericum origanifolium Willd. by Atomic Absorption Spectrometry

Atomic absorption spectrometry facilitates the reliable determination of mineral content during pharmaceutical quality control of medicinal plants. In the present work, measurable amounts of Fe, Ca, Cu, K, Mg, Mn, Na and Zn were detected in the leaves and flowers of Hypericum origanifolium Willd. through atomic absorption spectrometry. Mean heavy metal content in the flowers and leaves of H. origanifolium was, in descending order, Ca > Mg > K > Na > Fe. Ca was present in higher concentrations in the flowers (11157.24 ppm) and leaves (20132.24 ppm) of titled plant. Our results reveal that flowers are less suitable as target plant parts for metal accumulation than leaves.

Characterization of the volatile compounds and anatomical features in commercial samples of Echinodorus plant species

Echinodorus grandiflorus and Echinodorus macrophyllus are medicinal plants that are widely used in Brazilian folk medicine. The aims of this study were to evaluate the effect of oven drying with ventilation on the chromatographic profile of volatile compounds and to compare the leaf anatomy and volatile compounds of different commercial E. macrophyllus (Kunth) Micheli and E. grandiflorus Mich. Samples. The components found in fresh and dried samples were extracted by SPME and analysed by GC-MS, and the anatomical features of the leaves were observed microscopically. A total of 46 compounds were identified; five compounds were present in the dried and fresh samples of E. grandiflorus and all of the commercial samples. The anatomy analyses confirmed the authenticity of the species. Apparent differences in the volatile composition between the species were observed, allowing the identification of chemical marker. The results showed that commercial establishments do not conform to regulations, and the techniques used were effective for the characterization of volatile compounds and for quality control of medicinal plants.

The quality of wild Salvia miltiorrhiza from Dao Di area in China and its correlation with soil parameters and climate factors

Salvia miltiorrhiza is a frequently used herb in traditional Chinese medicine, and tanshinone IIA (Tan IIA) and salvianolic acid B (Sal Acid B) are two major extracts obtained from its dried root. The quality of herbal ingredients can be affected by environmental factors. To evaluate the quality of wild S. miltiorrhiza and investigate the influence of soil constituents and parameters as well as climatic conditions and factors on the content of Tan IIA and Sal Acid B. We collected samples in 12 natural locations in the Dao Di area in China, the area in which S. miltiorrhiza grows, that results in a distinctive higher quality of medicinal materials from the harvested plant. The concentrations of Tan IIA and Sal Acid B were measured by high-performance liquid chromatography (HPLC). Soil total carbon, total nitrogen, available nitrogen, available phosphorus, available potassium, and particle size distribution were determined. We also collected climate data using ArcGIS from the WorldClim database, and correlation tests, redundancy, and regression analyses were conducted to analyse the relationship and cluster the samples according to their chemical profile. The content of Tan IIA and Sal Acid B in most of the samples was significantly different (P < 0.05). Soil available phosphorus was considered as a key factor that influenced the quality of wild S. miltiorrhiza, and we found a significant negative association between the concentration of Tan IIA in roots and soil available phosphorus. Moreover, the accumulation of Tan IIA in S. miltiorrhiza was also significantly associated with precipitation in April, May, and October, maximum temperature in January, and standard deviation of temperature seasonality. There was no significant correlation between the content of Sal Acid B and ecological factors. In addition, samples collected from Mengshan, Hexian, and Lushi locations were rich in Tan IIA and tended to cluster together, whereas samples collected from Longquan and Huoshan locations tended to cluster and were poor in Tan IIA. The Tan IIA content in samples collected from southern Anhui was significantly lower than that in other Dao Di locations. The content of Tan IIA was related more to the soil than the temperature. Compared with Tan IIA, Sal Acid B was less influenced by soil and climate factors. The findings of this study may provide helpful references for quality control of medicinal plants that exert pharmacological effects in humans.

Box-Behnken supported development and validation of robust HPTLC method: an application in estimation of punarnavine in leaf, stem, and their callus of Boerhavia diffusa Linn.

Boerhavia diffusa (BD) Linn. (Nyctaginaceae) is one of the most commonly used herbs in the Indian traditional system of medicine for the urinary disorders. The aim of the current investigation was to carry out initiation, development, and maintenance of BD callus cultures and quantitative estimation of punarnavine in plant and callus extracts. Leaves and stem of BD were used as explant for the tissue culture studies using Murashige and Skoog (MS) basal medium. MS Media comprising 2,4-Dichlorophenoxy acetic acid (2,4-D) (1ppm) and 2,4-D (1ppm) + Indole-3-acetic acid (IAA) (1.0ppm) were found to yield friable callus from leaf explant; similarly, 2,4-D (0.3ppm) + IAA (0.75ppm) + Kinetin (0.3ppm) and 2,4-D (0.5ppm) + Naphthalene acetic acid (NAA) (1.5ppm) + Kinetin (0.3ppm) were found to yield friable callus from the stem explant. High-performance thin-layer chromatography method was been developed for the quantitative estimation of punarnavine (R f = 0.73) using mobile phase containing toluene: ethyl acetate: formic acid in the ratio (7.0:2.5:0.7, v/v/v) at 262nm. The validated method was found linear (r 2 = 0.9971) in a wide range (100-1000ng spot-1), precise, accurate, and robust. The values of limit of detection, LOD = 30.3ng spot-1, and limit of quantification, LOQ = 100.0ng spot-1. The robustness of the method was proved by applying the Box-Behnken design (BBD). The developed method found appropriate for the quality control of medicinal plants containing punarnavine as a constituent.

Quality assessment of Moringa seed shells based on fingerprinting using HPLC-DAD

A fingerprint analysis method was established for the quality control of Moringa seed shells by high-performance liquid chromatography with diode array detection (HPLC–DAD). The HPLC–DAD separation was performed on a Thermo Hypersil Gold C18 (4.6 mm × 250 mm, 5 μm) column by gradient elution with acetonitrile–water as mobile phase. The fingerprint of Moringa seed shells was established with good precision, reproducibility, and stability obtaining within 60 min, and 13 common peaks in the fingerprint were designed. Similarity analysis, principal component analysis (PCA), and hierarchical clustering analysis (HCA) were carried out to analyze the obtained fingerprints. The similarity among 11 batches of samples in addition to No. 5 and 6 was no less than 0.92. Eleven samples could be classified into 2 clusters. The HPLC fingerprint technology and application of chemical pattern recognition can provide a more comprehensive reference for the quality control of medicinal plants.

Sensitive Determination of C-Alkylated Flavonoids by HPLC-ESI-MS/MS Using Multiple Reaction Monitoring Approach: Pseudarthria hookeri as a Case Study.

One of the major problems with the formulation of herbal medicines is the quality control of plant material to ensure its efficacy and safety. Quality control of medicinal plants requires analysis of many bioactive compounds present in the plant. C-alkylated flavonoids are an important bioactive subclass of flavonoids. A simple, rapid, sensitive and selective method is presented here for the quantification of bioactive C-alkylated flavonoids. This is the first quantitative method for analysis of C-alkylated flavonoids based on the multiple reaction monitoring (MRM) approach so far. This study focuses on method development for quantification of bioactive C-alkylated flavonoids. Quantification of a total of five C-alkylated flavonoids was done employing the MRM approach on an HPLC-QqQ-MS instrument. LODs and LOQs for quantified flavonoids were in the range of 0.41-1.32 and 1.23-3.96ng/mL, respectively. Linear calibration curves between 25 and 1500ng/mL were obtained with the regression coefficients of ≥0.996. Accuracy (% bias) and precision (% RSD) of the analyses were found to be less than 5%. Developed HPLC-ESI-MS/MS can be employed as a quality control method of plant raw materials.

Assessment of ultrasound-assisted extraction combined with supramolecular solvent-based microextraction for highly sensitive cadmium determination in medicinal plant sample by TS-FF-AAS

A new analytical method exploiting supramolecular solvent-based microextraction (SUPRAS) combined with ultrasound-assisted extraction to preconcentrate cadmium from medicinal plant, with further determination by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS), is proposed. The proposed method is based on the cadmium ultrasound-assisted extraction from Ginkgo biloba L. leaf samples with diluted acid (0.10 mol L−1 HNO3), followed by the metal complexation with diethyl dithiophosphate and preconcentration using a supramolecular solvent composed of inverted hexagonal aggregates of dodecanoic acid arranged in tetrahydrofuran/water medium. The limits of detection (LOD) and quantification (LOQ) were found to be 0.11 μg L−1 and 0.36 μg L−1, respectively. Intraday and interday precision assessed in terms of relative standard deviations (RSD, %) were lower than 8.50% to 0.70, 1.75 and 5.00 μg L−1 cadmium solutions. The efficiency of ultrasound-assisted extraction was comparable to microwave-assisted digestion and the method accuracy was checked by analysis of certified reference material (Tomato Leaves, SRM 1573a). Samples of Ginkgo biloba L. were analyzed and cadmium contents between 0.21 and 0.33 μg g−1 were found, thereby showing clearly the importance of investigating toxic metals in medicinal plants. The proposed method is simple, highly sensitive, environmentally friendly and has great potential to be applied in the quality control of medicinal plants aiming trace cadmium determination.

EMERGING TRENDS IN QUALITY CONTROL OF HERBAL MATERIALS

The therapeutic use of medicinal plants gained considerable momentum in the world during the past few decades. Traditional medicines, which are mostly based on the herbal raw materials growing in their respective regions, were used by over 70 percent of the world population as per WHO. The reason for their popularity was due to non-availability of modern medicines in the rural areas and also due to the unaffordability of modern medicines due to their high cost. Quality control of medicinal plants for use in these Traditional medicines has always been a challenge for the scientists working in this field. In our country, with the awareness growing among the people about the safety of Ayurvedic and Herbal medicines / cosmetics, the quality control testing of both raw herbal ingredients and finished formulations was seriously undertaken both by the academic / research institutions and the herbal drug manufacturers.

Quantification of the total amount of black cohosh cycloartanoids by integration of one specific 1H NMR signal

Quantitative analysis is an important field in the quality control of medicinal plants, aiming to determine the amount of pharmacologically active constituents in complex matrices. Often biological effects of herbal drugs are not restricted to single compounds, but are rather caused by a number of often biogenetically related plant metabolites. Depending on the complexity of the analyzed plant extract, conflicts between accuracy, such as total content assays using photometric or colorimetric methods, and comprehensiveness, e.g. quantification of one or a few lead compounds can occur. In this study, we present a qHNMR approach determining the total amount of cycloartanoids in black cohosh (Actaea racemosa) rhizomes. Perdeuterated methanol containing 1,2,4,5-tetrachloro-3-nitrobenzene as an internal standard was used for extraction. Amounts of cycloartanoids were then measured by integrating 1H NMR signals of all cycloartenoids’ H-19 exo protons. Due to their unusually low chemical shifts, these signals are well separated from all remaining signals in crude extracts. Thus, accurate (recovery rates of 99.5–102.5%) and precise (relative standard deviations below 2.5%) quantification of cycloartanoids was accomplished. To the best of our knowledge, this is the first example of a quantification of the total amount of a pharmacologically relevant compound class by integration of one 1H NMR signal characteristic for all members of this particular compound class. Additionally, we propose a new term and unit for the evaluation of medicinal plants and herbal medicinal products: the “specific partial amount of substance” of pharmacologically active constituents, indicated in mmol/g.

Roles of &amp;lt;italic&amp;gt;SmCOI1&amp;lt;/italic&amp;gt; in pest resistance and secondary metabolism regulation based on &amp;lt;italic&amp;gt;Salvia miltiorrhiza&amp;lt;/italic&amp;gt; Bunge genome

Herb genomics is of great significance to studies of molecular breeding, secondary metabolite regulation, and quality control of medicinal plants. We isolated SmCOI1 gene from the medicinal plant Salvia miltiorrhiza Bunge by screening genome databases and analyzed the structure and expression pattern of this gene. For functional analysis, we down-regulated SmCOI1 expression in S. miltiorrhiza ( iCOI1s ) via RNA interference. Tests conducted to examine pest resistance revealed that leaf damage scores of iCOI1s were much higher than those of wild-type plants, whereas the expression of defense genes ( NPR1 and WRKY70 ) was significantly reduced in iCOI1s . Major secondary metabolite contents of S. miltiorrhiza (rosmarinic acid, salvianolic acid B, cryptotanshinone, and tanshinones IIA) were significantly reduced compared with those of wild-type plants. Furthermore, the expression of key genes involved in tanshinones and salvianolic acid biosynthesis pathways ( HMGR , GGPPS , CPS , KSL , CYP76AH1 , C4H , RAS , and HCT ) was also down-regulated in iCOI1 plants. Our results indicated that SmCOI1 plays a critical role in pest resistance and secondary metabolism regulation in S. miltiorrhiza , paving the way for the breeding of high-quality medical plants.

Front Cover: High‐performance thin‐layer chromatography: An economical alternative for the quality control of medicinal plants and derived products

Front Cover: High‐performance thin‐layer chromatography: An economical alternative for the quality control of medicinal plants and derived products

High‐performance thin‐layer chromatography: An economical alternative for the quality control of medicinal plants and derived products

AbstractCurrently, delicious and essential items are intentionally diluted to gain higher profit in the market. Awareness about the quality of naturally derived products such as food, nutrients, cosmetics, and drugs has increased. An economical method for their quality assessment is needed. In this regard, high‐performance thin‐layer chromatography is an inexpensive, fast, and reproducible technique for quality control. The basics of thin‐layer chromatography and high‐performance thin‐layer chromatography have been reviewed previously, but a comprehensive compilation of its applications is lacking. The current review focuses on high‐performance thin‐layer chromatography based analytical methods for the quality assessment of various plant species, plant materials, plant‐derived products, food and nutrients, and cosmetics (natural origin). This review covers all aspects of high‐performance thin‐layer chromatography and will prove fruitful for research and development in academia and industry.

Some triterpenic compounds in extracts of Cecropia and Bauhinia species for different sampling years

The aim of this paper is to provide an overview on the chemical composition of triterpenes in widespread used folk medicine species, through the development and validation of eleven compounds using HPLC-UV detection. The compounds were separated using isocratic elution, on a reverse phase column (Kinetex C18, 250mm×4.6mm, 5μm) with mobile phase consisted of acetonitrile:tetrahydrofuran (90:10, v/v), flow-rate of 0.5ml/min and detection in 210nm. Diverse validation parameters were successfully evaluated. The samples of Bauhinia variegata L., B. variegata var. candida Voigt, Fabaceae, Cecropia palmata Willd. and C. obtusa Trécul, Urticaceae, collected in 2012, 2013 and 2014 from Amazon were treated with two different solvents (ethyl acetate and chloroform) and analyzed by the proposed method. Stigmasterol, lupeol, β-sitosterol, β-amirin and α-amirin were found in all the studied plants. Highlighting the presence of oleanolic acid, maslinic acid in C. obtusa and C. palmata extracts, erythrodiol only in C. palmata, stigmasteol in B. variegata and α-amirin in B. variegata var. candida. Overall, ethyl acetate showed better performance as the extractor solvent than chloroform. Moreover, it could be used for the quality control of medicinal plants and to assess potential marker compounds.