ABSTRACT
Objective In order to verify an alternative method for the skin corrosion test by using transcutaneous electrical resistance ( TER) test, and to optimize the implementation criteria in OECD TG 430 procedure. Methods According to the OECD TG 430 procedure, Wistar rat skin was used to test the TER values of 16 reference chemicals, and selected the most optimal standard via different implementation criteria. The program B was chosen to make inter-laboratory comparison between 5 laboratories by testing 11 chemicals, which were identified as the optimal standard. Results After the TER test, the result of corrosion test of 16 chemicals were accordant with the reference data ( Kappa value＝0. 64). The program B was the most optimal implementation criteria, and the specificity was 66. 7% and sensitivity was 100%. There were no significant differences between the corrosion estimations of 5 laboratories, and the concordance rate of the 5 laboratories was 72. 7%. Conclusions Transcutaneous electrical resistance (TER) test is an feasible and efficient tool for skin corrosion testing, and may become a good interim test to replace the in vivo test with this ex vivo test in cosmetics chemical safety assessment, thus, to reduce the animal usage in our country.
ABSTRACT
A multi-residue analysis method was developed for the determination of 38 kinds of pesticides in nuts (almonds, peanuts, cashew nuts and walnuts) by QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry.The pesticide residues were extracted with acetonitrile.The extract was cleaned up with PSA, C18 and Oasis PRiME HLB, and then analyzed by UPLC-MS/MS with multiple reaction monitoring (MRM) mode.External standard method was employed to quantify.The limits of detection (LODs, S/N=3) of this method were between 0.01 and 10 μg/kg, and the limits of quantitation (LOQs, S/N=10) were between 0.05-20 μg/kg.All of the tested pesticides showed good linear relationship (r>0.991).The practical samples were determined at three spiked levels and the average recoveries were between 51.0% and 126.0%.The RSDs were less than 20%.This method was simple, sensitive and accurate, and could be used for the routine analysis of pesticide residues in nuts.
ABSTRACT
<p><b>OBJECTIVE</b>To study the chemical constituents of the roots of Phlomis medicinalis.</p><p><b>METHOD</b>The compounds were isolated and repeatedly purified by macroporous resin, silica gel column chromatography, TLC and PREP-HPLC. Their structures were elucidated by physical and chemical properties and NMR spectra.</p><p><b>RESULT</b>Two iridoid glucosides were obtained and elucidated as 7-epilamalbide (1), chlorotuberoside (2).</p><p><b>CONCLUSION</b>Compound 1 was a new compound, compound 2 was isolated from the plant for the first time.</p>
Subject(s)
Glucosides , Iridoid Glucosides , Iridoids , Magnetic Resonance Spectroscopy , Phlomis , Chemistry , Plant Roots , ChemistryABSTRACT
<p><b>OBJECTIVE</b>To apply the near infrared spectroscopy in quality control for excipients of traditional Chinese medicine (TCM).</p><p><b>METHOD</b>A new type of transmittance and reflectance integration sphere accessory and a transmittance accessory were used to collect the spectra of processed honey and rice wine, respectively. Determination method of reducing sugar and ethanol in processed honey were established with partial least squares (PLS).</p><p><b>RESULT</b>The correlation coefficients (r), the root mean square error of calibration (RMSEC) and the root mean square error of prediction (RMSEP) of the proposed models were 0.9593, 1.00% and 1.19% for reducing sugar; 0.9529, 0.17% and 0.24% for ethanol.</p><p><b>CONCLUSION</b>The proposed method is fast, non-destructive, simple and accurate, and can be applied to at-spot detection,</p>
Subject(s)
Excipients , Chemistry , Honey , Medicine, Chinese Traditional , Oryza , Chemistry , Quality Control , Spectroscopy, Near-Infrared , Methods , WineABSTRACT
Objective To study the chemical constituents of Heterosmilax yunnanensis.Methods The compound was isolated and repeatedly purified with chromatography and the structure was elucidated by physico-chemical properties and spectral analysis.Results A new compound was isolated and identified.Conclusion This compound is a novel compound with structure of 1,3,6,7-tetrahydroxy-xanthone-3-O-?-D-glucopyranoside,mamed heterosmioside A.
ABSTRACT
Objective To study the chemical constituents in the roots of Phlomis medicinalis.Methods The compound was isolated and repeatedly purified by macroporous resin,silica gel column chromatography,TLC,and Prep-HPLC.Its stracture was elucidated by physical and chemical properties and NMR spectra.Results One iridoid glucoside was obtained and elucidated as 8,10-dehydropulchelloside.Conclusion The compound is a new one.
ABSTRACT
Objective To study the chemical constituents of Phlomis medicinalis.Methods The constituents were isolated and purified by various modern chromatography techniques and the structures were elucidated by physicochemical properties and spectral analyses.Results Ten compounds were obtained and elucidated as 1-dehydroxyshanzhigenin methyl ester(Ⅰ),notohamosin A(Ⅱ),verbascoside(Ⅲ),3,4-dihydroxyphenyl ethanol(Ⅳ),succinic acid(Ⅴ),sucrose(Ⅵ),2,6-difructose(Ⅶ),butyl-?-D-fructopyanoside(Ⅷ),D-glucose(Ⅸ),and D-fructose(Ⅹ).Conclusion All the compounds are isolated from this plant for the first time,compound Ⅱ is obtained from the plants of Phlomis Linn.for the first time,and compound Ⅰ is a new one.
ABSTRACT
Objective To investigate the chemical constituents of Balanophora simaoensis. Methods Chromatography and spectra were used to isolate the constituents and elucidate their structures. Results Four compounds were isolated from whole plant of B. simaoensis and elucidated as methylconiferin (Ⅰ), butylconiferin (Ⅱ), 4-O-?-D-glucopyranosyl confieryl aldehyde (Ⅲ), and brevifolin (Ⅳ), respectively. Conclusion Butylconiferin is a new compound.
ABSTRACT
Objective: To study the specificity of the determination method for catechin and epicatechin in Catechu. Method: Contents of catechin and epicatechin in 7 kinds of crude drugs and 3 kinds of preparations of Catechu were determined. Results: As sampling 100 times as much as Catechu, catechin and epicatechin could be both detected in Semen Arecae, and catechin could be detected in Radix et Rhizoma Rhei, Herba Ephedrae and Radix Sanguisorbae. Conclusion:This method can be used for the quality control of Catechu and its preparations and is of specificity.
ABSTRACT
AIM: To study Cordyceps sinesis and its cultured mycelia by HPLC.METHODS: An HPLC established for the fingerprints of cordyceps sinensis and its cultured mycelia was performed on an Agilent C18(4.6 mm ? 25 mm,5 ?m)as column and acetonitrile-0.1% phosphoric acid solution in gradient as mobile phase.The flow rate was 0.5 mL/min,and the detection wavelength was set at 260 nm.RESULTS: There were 6 common peaks in HPLC fingerprint of Cordyceps corensis and its cultured mycelia,three of which were determined as uracil,adenosine,cordycepin.CONCLUSION: The method can be used for the study of fingerprints of cultured mycelia.
ABSTRACT
AIM:To improve the quality control standard based on 3 kinds of Radix Isatidis preparations-Radix Isatidis syrup,chewable tablet and granules. METHODS: A TLC method was established for iden tification of with Isatidis indigotica RS,Vleucine CRS and Arginine CRS as the references.A HPLC method was developed for the determination of adenosine and igoitrin in Radix Isatidis Preparations,with DIKMA Diamonsil C_(18) column(5 ?m,200 mm?4.6 mm id),a mixure of acetonitrile-water-triethylamine(10∶90∶0.2,using glacial acetic acid to adjust to pH 5.2)-water(85∶15) as the mobile phase.The detection wavelength was set at 245 nm. RESULTS: Isatidis indigotica,Vleucine and Arginine were detected in all the preparations.The contents of adenosine and igoitrin varied greatly in tested samples from different pharmaceutical enterprises. CONCLUSION: The above methods are simple,accurate,and suitable for the quality control of Radix Isatidis Preparations.
ABSTRACT
AIM: To study the application of near infrared spectroscopy for quality control of in-process Wuji Baifeng Pill(Gallus Domesticus,Colla Cornus cervi,Carapax Trionycis,Otheca Mantidis,Radix et Rhizoma Ginseng,etc.). METHODS: Qualitative and quantitative methods for analysis of in-process product was developed by diffuse reflectance near infrared spectroscopy combined with chemometrics.Spectra of 95 samples of Tongren Wuji Baifeng Pill in-process and 19 raw material negative in-process products were collected.Similarity match model was built on the basis of spectra of 75 batches of qualified in-process products.Using this model,the similarity match values of other samples were calculated.Multivariate calibration models for paeonin and water content in in-process product were developed with partial least square algorithm. RESULTS: The results showed that the proposed similarity match model could reflect the quality characteristic of Tongren Wuji Baifeng Pills in-process and reveal the absence and presence of raw materials.The correlation coefficients of the calibration model were within 0.965 7 and 0.992 1 while the values of root mean square error of prediction were 0.005 5% and 0.45%,respectively. CONCLUSION: The experiment shows that the established method is accurate,fast and non-destructive,and can be applied to on-line detection.
ABSTRACT
AIM: To affirm marker peaks for the fingerprint chromatography of Shengmai Injection. METHODS: LC-MS/MS method was used, with a Waters symmetryshield TM RP_ 18 column(4.6 mm?250 mm; 5.0 ?m), acetonitrile-water as a mobile phase, The detection wavelength was at 203 nm. Ion trap mass spectrum. RESULTS: Affirming marker peaks for fingerprint chromatography of Shengmai Injection and 10 marker peaks were affirmed. CONCLUSION: The method can affirm marker peaks for the fingerprint chromatography of Shengmai Injection. It is simple, accurate, and has practicality.
ABSTRACT
AIM: To establish a method of simultaneous determining 4 components in Shengmai Injection (Radix et Rhizoma Ginseng Rubra,Radix Ophiopogonis,Fructus Schisandrae Chinensis). METHODS: Four components:ginsenoside Rg_1、ginsenoside Re、ginsenoside Rb_1 and schisandrin in Shengmai Injection were determined simultaneously by HPLC, using a waters symmetryshield TMRP_(18) column(4.6 mm?250 mm; 5.0 ?m),acetonitrile-water as a mobile phase. The detection wavelength was at 203nm. RESULTS: The relationship between the concentrations and the peak areas of ginsenoside Rg_1、ginsenoside Re、ginsenoside Rb_1 and schisandrin was linear respectively.The RSD of precision,repeatability and recovery were all less than 1%. CONCLUSION: The method is simultaneous determination for four components in Shengmai Injection,and can be applied to the quality control of Shengmai Injection.
ABSTRACT
Objective: To study the distribution of flavonoids among the plants for medicinal use of Selaginella . Methods: HPCE analysis was carried out on the ethyl acetate extracts of 18 Selaginella plants (from 11 species), using MECC separation model. Results: HPCE fingerprints of 18 Selaginella plants were established with quercetin as interanl standard and relative migration time and relative peak area as parameters. Conclusion: The contributions of flavonoids has not only generity, but also difference among the tested samples.