This study aims to explore the evaluation model for the proficiency testing of heavy metal and harmful element residues in pharmaceuticals,and to provide reference for the proficiency testing program and proficiency testing result in the field of residue analysis. The proficiency test result of cadmium determination in honeysuckle as an example. The algorithm A,NIQR,and Horwitz function are used to calculate the assigned value and the standard deviation. Z was obtained at the same time. If | Z | ≤2,the result is satisfactory. If 2< | Z | <3,the result is questionable. If | Z | ≥3,the result is unsatisfactory. In addition,the median value is the assigned value,and deviation(D%) is used. If D% is not more than 16%,the result is satisfactory; if D% is more than 16%,the result is unsatisfactory. After analysis,in the results of questionable or dissatisfied laboratories calculated by algorithm A and NIQR,the deviation error of some data is within the scope of the standard. In the results of the satisfactory laboratory evaluated by the Horwitz function,some data deviation errors far exceed the standard range. The evaluation result of the D% meets the requirements. According to heavy metal and harmful element trace analysis methods,this study is the first to apply D% to the evaluation of the detection ability of heavy metals and harmful elements in pharmaceuticals. This method makes the evaluation result more reasonable,and has important reference significance for the evaluation of other proficiency test results.
Cadmium ; analysis ; Laboratories ; Laboratory Proficiency Testing ; Lonicera ; chemistry ; Pharmaceutical Preparations ; standards ; Plant Preparations ; standards ; Trace Elements ; analysis

With the improvement of living standard,the theory of " medicine and food homology" has developed rapidly in the field of diet,medicine and health preservation. In recent years,many literatures have been reported on the active ingredients and pharmacological effects of medicinal and edible plants,but relatively few reports have been reported on their safety investigation. Therefore,to further evaluate the quality and safety of medicinal and edible plants,Astragali Radix,Codonopsis Radix and Laminariae Thallus were selected as our research objects in this study. Moreover,the pollution level and the potential health risk of heavy metals were deeply assessed in different types of medicinal and edible plants. Especially,the contents of chromium,copper,arsenic,cadmium,mercury and lead in these three herbs were determined by inductively coupled plasma mass spectrometry( ICP-MS),and their health risk level was evaluated by target hazard coefficient method. The results showed that under the international heavy metal limit standard( ISO 18664-2015,GB 2762-2017),the over-standard rates were 25%,77% and 100% in 16 batches of Astragali Radix,26 batches of Codonopsis Radix and 9 batches of Laminariae Thallus,respectively. Besides,the values of target hazard quotients( THQ) for adults and children are 0. 028 244,0. 063 505 and 0. 014 485,0. 032 568 in Astragalus membranaceus and Codonopsis pilosula,respectively,which were higher than the standard values of 0. 02 and 0. 011 25. While,the total heavy metals THQ values for adults and children are 0. 023 734 and 0. 020 287 in Laminariae Thallus,which were much higher than the standard values of 0. 008 0 and 0. 007 5. However,the CR values of As,Cd and Pb in the three herbs were lower than 1×10~(-6). Above results indicated that those six harmful elements have certain health hazards to the exposed population,but there is no potential carcinogenic effect. It can be seen that,there were still presence of the pollution of harmful elements,and it is necessary to establish the reasonable limit standards and quality control methods of medicinal and edible plants in time.
Adult ; Astragalus propinquus ; Child ; Codonopsis/chemistry* ; Drugs, Chinese Herbal/chemistry* ; Humans ; Laminaria/chemistry* ; Metals, Heavy/analysis* ; Plant Preparations/chemistry* ; Plants, Edible/chemistry* ; Plants, Medicinal/chemistry* ; Risk Assessment

This study aimed to analyze the residues of aflatoxin B_1( AFB_1) in Ziziphi Spinosae Semen from different producing areas and to assess the health risk of aflatoxin B_1 residue based on the obtained data. A total of 72 samples of Ziziphi Spinosae Semen from different areas were detected by IAC-HPLC-FLD. Based on the data of AFB_1 pollution,a probabilistic assessment model with Monte Carlo simulation was developed. Then,the risk assessment of AFB_1 exposure by Ziziphi Spinosae Semen intake was carried out by MOE( margin of exposure). The results showed that 32 out of 72 of samples( 44. 4%) were found to be contaminated with AFB_1,and the average and maximum concentration of AFB_1 in samples was 5. 42 μg·kg~(-1) and 55. 09 μg·kg~(-1),respectively. After health risk assessment,the average and 97. 5%( 90% confidence interval) exposure level of daily exposure of AFB_1 by Ziziphi Spinosae Semen intake were 0. 008 6( 0. 008 1-0. 009 2) and 0. 057 3( 0. 053 2-0. 061 4) μg·kg~(-1)·d~(-1),respectively. The results showed common use of Ziziphi Spinosae Semen had low level of risk associated with AFB_1. However,the high consumption of Ziziphi Spinosae Semen showed a higher risk than common intake,requiring attention. This study laid a foundation for clinical safe prescription of Ziziphi Spinosae Semen.
Aflatoxin B1/analysis* ; Chromatography, High Pressure Liquid ; Drug Contamination ; Plant Preparations/analysis* ; Risk Assessment ; Ziziphus/chemistry*

The quality of honeysuckle has always been an important factor in industrial development. Flowering is one of the elements for the variation of the effective components in honeysuckle. We can conveniently recognize whether the commodity is mixed with blossomed honeysuckle in the form of medicinal material. However,it is hard to identify whether the products are mixed with blossomed honeysuckle in the form of powdersince visual identification traits are missing. Therefore,this study aims to seek an effective method of odor-based distinguish for identifying the quality of honeysuckle powder in different ratios by using Heracles Ⅱ ultra-fast gas phase electronic nose.The powdered samples were prepared with flower buds and fully blooming flowers in different proportion. Gas chromatograms of the powder were obtained by HeraclesⅡ ultra-fast gas phase electronic nose. Through analyzing the data of chromatograms,we have concluded that the qualitative results of the prepared powder were almost the same,and there existed differences in the components content. Meanwhile,the hexanal odor appeared to be the critical factor in identifying honeysuckle powder quality among the flavor of all possible compounds. Also,we have applied PCA,DFA and CQ to identify and classify the variety of the powder based on the chromatogram data. Finally,it is realized that the powder was rapidly identified and classified into three grades based on the proportion of flowering honeysuckle. The predicted concentration value for the first class is less than 3,the value of is not less than 3 and less than 5 for the second class,and more than 5 for the third class. In summary,the results obtained by the study suggest that Heracles Ⅱ ultra-fast gas phase electronic nose analysis can be used as a rapid identification method for the quality of honeysuckle powder. At the same time,it can provide a reference for the quality classification of honeysuckle based on flowering degrees.
Electronic Nose ; Flowers/chemistry* ; Lonicera/chemistry* ; Odorants/analysis* ; Plant Preparations/analysis* ; Powders/analysis* ; Quality Control

OBJECTIVEAging is associated with the development of diseases because of immunosuppression and altered functioning of the neuroendocrine system. The medicinal properties of Morinda citrifolia L. have been widely exploited for the treatment of age-associated diseases. This study aims to investigate the in vitro and in vivo effects of noni (M. citrifolia) fruit juice (NFJ) on neuro-immunomodulation in the lymph node lymphocytes of F344 rats.

METHODSLymphocytes isolated from axillary and inguinal lymph nodes of young (3-4 months) and old (18-21 months) rats were treated in vitro with different concentrations (0.0001%, 0.01%, and 1%) of NFJ for a period of 24 h. In the in vivo study, old (16-17 months) male F344 rats were treated with 5 mL/kg body weight of 5%, 10% and 20% of NFJ, twice a day, by oral gavage, and lymph node lymphocytes were isolated after 60 d. Concanavalin A (Con A)-induced lymphocyte proliferation, interleukin-2 (IL-2) and interferon-γ (IFN-γ) production and expression of intracellular markers, such as phospho-extracellular signal-regulated kinase (p-ERK1/2), phospho-cAMP response element-binding protein, phospho-protein kinase B (p-Akt), phospho-tyrosine hydroxylase (p-TH), phospho-nuclear factor of κ light polypeptide gene enhancer in B-cells inhibitor-α (p-IκB-α) and phospho-nuclear factor-κB (p-NF-κB p65 and p50) were examined in the lymphocytes of lymph nodes.

RESULTSNFJ increased Con A-induced lymphocyte proliferation, IL-2 and IFN-γ production, and p-ERK1/2 expression both in vitro and in vivo. In in vivo NFJ-treated old rats, lymph node lymphocytes showed increased expression of p-TH and Akt, nitric oxide production and decreased expression of p-NF-κB p65 and p50.

CONCLUSIONThese results suggest that the immunostimulatory properties of NFJ are facilitated through intracellular signaling pathways involving ERK1/2, Akt and NF-κB.

Adjuvants, Immunologic ; metabolism ; Aging ; immunology ; metabolism ; Animals ; Cell Proliferation ; Fruit ; chemistry ; metabolism ; Fruit and Vegetable Juices ; analysis ; Humans ; Interleukin-2 ; immunology ; Lymph Nodes ; cytology ; immunology ; Lymphocytes ; cytology ; immunology ; Male ; Morinda ; chemistry ; metabolism ; NF-kappa B ; immunology ; Plant Preparations ; metabolism ; Rats ; Rats, Inbred F344 ; Transcription Factor RelA ; immunology

The raw and processed roots of Plygonum multiflorum Thunb (PM) are used to treat different diseases in clinical practice. In order to clarify the influence of processing, a comparative study of chemical substance analysis was carried out. As the xenobiotics with a high enough exposure in target organs being considered as the potential effective or toxicity components, an in vivo study was also implemented to characterize the constitutes and metabolites, and meanwhile, the factor of compatibility with black bean were also considered. As a result, a total of 148 compounds were detected in PM extracts and more than 40 compounds were only detected in the processed products, which were probably new components produced during the steaming process. In in vivo study, 7 prototype components and 66 metabolites were detected or tentatively identified, 24 of which were reported for the first time. Our results indicated that processing greatly changed the chemical composition of PM and influenced the disposition of the compounds in vivo. To the best of our knowledge, this was the first global comparative study of raw and processed PM. These results expanded our knowledge about the influence of processing of PM and provided the essential data for further efficacy or toxicity studies.
Animals ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; metabolism ; Male ; Plant Preparations ; chemistry ; isolation & purification ; metabolism ; Plant Roots ; chemistry ; Polygonum ; chemistry ; Rats ; Rats, Sprague-Dawley ; Spectrum Analysis

Local healthcare providers often question the possible steroidal activity of traditional Chinese medicine (TCM) herbs or herbal products and implicate them as a cause for adrenal insufficiency or Cushing's syndrome in patients with a history of TCM intake. We conducted a comprehensive database search for evidence of potential glucocorticoid, mineralocorticoid, androgenic or oestrogenic activity of herbs or herbal products. Overall, there are not many herbs whose steroidal activity is well established; among these, most cases were based on preclinical studies. Liquorice root may cause pseudoaldosteronism through interference with the steroidogenesis pathway. Although ginseng and cordyceps have some in vitro glucocorticoid activities, the corroborating clinical data is lacking. Deer musk and deer antler contain androgenic steroids, while epimedium has oestrogenic activity. On the other hand, adulteration of herbal products with exogenous glucocorticoids is a recurrent problem encountered locally in illegal products masquerading as TCM. Healthcare providers should stay vigilant and report any suspicion to the relevant authorities for further investigations.
Androgens ; analysis ; Animals ; Cordyceps ; Databases, Factual ; Deer ; Drugs, Chinese Herbal ; adverse effects ; analysis ; Epimedium ; Estrogens ; analysis ; Fatty Acids, Monounsaturated ; Glucocorticoids ; analysis ; Glycyrrhiza uralensis ; Humans ; Medicine, Chinese Traditional ; adverse effects ; Mineralocorticoids ; analysis ; Panax ; Plant Preparations ; analysis ; Risk ; Singapore ; Steroids ; adverse effects ; analysis ; Tissue Extracts

OBJECTIVEUsing Apocynum venetum as a model drug to prepare pulsed-release tablets based on diffusion, swelling, osmotic pressure mechanism and to evaluate the release characteristics.

METHODThe pulsatile release tablets were prepared by film coating methods using HPMC E5 and Eudragit The effect of formulation on pulsatile release of A. venetum was investigated.

RESULTThe pulsed-release tablet was prepared by a swelling layer coating which contains HPMC E5 and a controlled-release membrane containning Eudragit. The delayed release time of the tablets was (5.0 +/- 0.5) h.

CONCLUSIONThe pulsatile release characteristics of A. venetum pulsatile release tablets were confirmed in vitro.

Apocynum ; chemistry ; Delayed-Action Preparations ; chemistry ; Diffusion ; Drug Compounding ; methods ; Drugs, Chinese Herbal ; chemistry ; In Vitro Techniques ; Lactose ; analogs & derivatives ; analysis ; Methylcellulose ; analogs & derivatives ; analysis ; Osmotic Pressure ; Plant Leaves ; chemistry ; Polymethacrylic Acids ; analysis ; Solubility ; Tablets ; chemistry ; Time Factors

OBJECTIVETo develop and validate a HPLC-UV-ELSD method for the simultaneous determination of ginsenosides and epimedium flavonoids in rat urine after intravenous administration of Jiweiling freeze-dried powder.

METHODChromatographic separation was performed on a C18 HPLC column, with gradient elution of acetonitrile and water as mobile phase. An UV detector was used at detection wavelength of 220 nm. An evaporative light scattering detector (ELSD) was used at drift tube temperature of 80 degrees C and gas pressure of 172.4 kPa.

RESULTThe calibration curves were linear over the investigated concentration ranges with all correlation coefficients higher than 0.998. The a intra- and inter-day RSD were less than 9.1% and the relative errors were verage extraction recoveries for all compounds were between 88.67% and 101.2%. The within the range of -11.58% to 10.89%.

CONCLUSIONThe proposed method showed appropriate accuracy and selectivity and was successfully applied to the rat urine samples analysis of saponins and flavonoids after intravenous administration of Jiweiling freeze-dried powder, which may provide some references to the apprehension of the action mechanism and clinical application.

Animals ; Calibration ; Chromatography, High Pressure Liquid ; methods ; Epimedium ; chemistry ; metabolism ; Flavonoids ; urine ; Ginsenosides ; urine ; Phytotherapy ; Plant Preparations ; Rats ; Saponins ; analysis ; Ultraviolet Rays

OBJECTIVETo reveal the influence of harvest season and tree age on the content of taxol and 10-DAB III, and provide the basis for the harvest time of Taxus madia.

METHODBranches and leaves of the labeled 25 three-year-old plants and 25 five-year-old plants were collected every two months from March 26,2009 to January 26, 2010. Taxol and 10-DAB III content of different age and growth season of Taxus in branches were determined by HPLC.

RESULTTaxol and 10-DAB III content were significantly different in different harvesting age. The content of five-year-old plants was significantly higher than that of three-year-old plants. Taxol and 10-DAB III contents were significantly different in different harvesting season, and the highest content of taxol and 10-DAB III was 0.56, 0.32 mg x g(-1), respectively, in May.

CONCLUSIONThe May is the suitable harvest season for T. madia, but the suitable harvest age need further study which according to the main active component and biomass accumulation.

Antineoplastic Agents, Phytogenic ; analysis ; pharmacology ; Asteraceae ; chemistry ; Chromatography, High Pressure Liquid ; Paclitaxel ; analysis ; pharmacology ; Plant Preparations ; pharmacology ; Seasons ; Taxoids ; analysis ; pharmacology ; Taxus ; chemistry ; drug effects ; Trees ; chemistry