[Study on quality standard of Bufonis Venenum and its processed slice, toad venom powder].

Bufonis Venenum(toad venom) is prepared from the dried secretion of Bufo bufo gargarizans or B. melanostictus. Toad venom powder is one of the processed slices of crude material toad venom. In the present study, the global quality control method and standard of toad venom and its processed slice, toad venom powder were established, including TLC identification, characteristic chromatogram and QAMS by HPLC. The relative correction factor(RCF) was re-calculated and validated. The average RCFs of cinobufagin to gamabufotalin, bufotalin, bufalin and resibufogenin were considered for the determination of five bufadienolides in the samples. The total amount in the different batches of the dried samples varied from 4.06% to 17.0%. Referring to the revised methods for crude materials, the quality standard of toad venom powder was drafted including appearance description, TLC examination, characteristic chromatogram, water content and the total amount of five bufadienolides. The present investigation provided scientific evidences for the quality standard improvement of toad venom to be described in the next edition of Chinese pharmacopoeia(2020 edition).

[Simultaneous determination of sixteen mycotoxins contaminants in cogon rootstalk by QuEChERS-UPLC-QqQ mass spectrometry].

A method for the simultaneous determination of sixteen mycotoxins in cogon rootstalk was developed using ultra-performance liquid chromatography coupled with triple quadropole mass spectrometry(UPLC-QqQ-MS/MS). The samples were extracted with acetonitrile contained 1% acetic acid and purified by QuEChERS method. The separation was performed on an Agilent Eclipse Plus C18column by gradient elution using methanol and 0.01% aqueous formic acid as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization(ESI)source operated in positive ionization mode. The linear relationships of the sixteen mycotoxins were good in their respective linear ranges. The correlation coefficients(r)ranged among 0.996 2-1.000. The LOQs of the sixteen mycotoxins were between 0.03 and 186.68 µg•kg ⁻¹. The average recoveries ranged from 60.28% to 129.2% with relative standard deviations(RSDs)within 0.29%-11%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in cogon rootstalk.

[Quantitative analysis of nine ginsenosides in red ginseng using QAMS method based on high-resolution and reference chromatography of red ginseng].

Using reversed-phase high performance liquid chromatography, nine ginsenosides were simultaneously separated on an UltimateC18 column with high-resolution and high purity of each chromatographic peak. Adopting the QAMS quality evaluation model for traditional Chinese medicines, ginsenoside Rb1 was used as the internal reference substance, and the relative correction factors (RCFs) and the relative retention values (RTRs) of ginsenosides Rg1, Re, Rf, Rb1, Rc, Rb2, Rb3, Rd and 20 (S)-ginsenoside Rg3 to ginsenoside Rb1 were calculated individually. Through a series of methodology evaluations, and positioned by the red ginseng reference chromatograph and RTVs, nine ginsenosides in red ginseng were simultaneously assayed only by quantitative determined ginsenoside Rb1.

[Determination of 7 flavonol glycosides in Ginkgo biloba reference extract].

Six flavonol glycosides were isolated and calibrated from Ginkgo biloba extract, and then used to calibrate the content in 2 baiches of G. biloba reference extract, so was rutin. RSD values of rutin, kaempferol-3-O-rutinoside, kaempferol-3-O-rhamnoside-2-glu- coside, quercetin-3-O-rhamnop-yranosyl-2-O-(6-O-p-coumaroyl)-glucoside, kaempferol-3-O-rhamnopyranosyl-2-O-(6-O-p-coum-aroyl) - glucoside were around 1.1%-4.6%, nevertheless, RSD values of quercetin-3-O-glucoside and isorhamnetin-3-O-rutinoside were more than 5%. According to the results, the reference extract of G. biloba can be used as the substitute to determine rutin, kaempferol-3-O- rutinoside, kaempferol-3-O-rhamnoside-2-glucoside, quercetin-3-O-rhamnopyranosyl-2-O-(6-O-p-coumaroyl)-glucoside and kaempferol-3-0-rhamnopyranosyl-2-O-(6-O-p-coumaroyl)-glucoside instead of corresponding reference substances. So reference extract in place of single component reference in assay is feasible.

New oleanane-type triterpenoid saponins isolated from the seeds of Celosia argentea.

Three new oleanane-type triterpenoid saponins named celosins H, I, and J were isolated from the seeds of Celosia argentea L. Their structures were characterized as 3-O-ß-D-xylopyranosyl-(1 → 3)-ß-D-glucuronopyranosyl-polygalagenin 28-O-ß-D-glucopyranosyl ester, 3-O-ß-D-glucuronopyranosyl-medicagenic acid 28-O-ß-D-xylcopyranosyl-(1 → 4)-α-L-rhamnopyranosyl-(1 → 2)-ß-D-fucopyranosyl ester, and 3-O-ß-D-glucuronopyranosyl-medicagenic acid 28-O-α-L-arabinopyranosyl-(1 → 3)-[ß-D-xylcopyranosyl-(1 → 4)]-α-L-rhamnopyranosyl-(1 → 2)-ß-D-fucopyranosyl ester by NMR, MS, and chemical evidences, respectively. In our opinion, celosins H-J could be used as chemical markers for the quality control of C. argentea seeds.

Simultaneous determination of eleven flavonoid glycosides in ginkgo biloba leaves collected in different seasons by UPLC PDA method.

A new UPLC method was developed for the simultaneous determination of eleven characteristic flavonoid glycosides in Ginkgo biloba leaves. The natural occurrence of flavonoid glycosides in Ginkgo biloba leaves within one vegetative season was investigated for the first time. The analysis was performed on an Agilent ZORBAX Eclipse Plus C18 column (50 mm x 4.6 mm, 1.8 microm), the mobile phase A was acetonitrile, the mobile phase B was 0.4% phosphate aqueous solution in a gradient elution at a flow rate of 0.6 mL x min(-1), the detection was carried out at 360 nm. The result showed that eleven flavonoid glycosides had good linearity with good average recovery, separately. The method was proved to be accurate, rapid and good reproducible for the quality evaluation of Ginkgo biloba leaves, and provide an easy and rapid means for the quantitative analysis of flavonoid glycosides and their content fluctuation with seasons.

[Analysis on chemical compositions of Artemisia Argyi from Qichun of different years and moxa wool refined in different proportions].

The article aims at providing theoretical foundation for security of moxibustion through analyzing chemical compositions of Artemisia Argyi of different years from Qichun County, Hubei Province, and moxa wool refined in different proportions. Artemisia Argyi from Qichun on 2007, 2008 and 2009 were taken as raw materials, and processed into moxa wool with the proportions of raw material and product as 3 : 1, 5 : 1, 8 : 1 and 15 : 1, respectively. Essential oils of Artemisia Argyi and the refined moxa wool were extracted by steam distillation. Their chemical compositions were identified by gas chromatography-mass spectrometry (GC-MS) and calculated with semiquantitative method. The result showed that chemical compositions of Artemisia Argyi of different years and moxa wool refined in different proportions were almost the same, but their contents were with obvious difference. The relative content of volatile substances decreased with the age prolonged and a rise in the proportion of the refined moxa wool, while the involatile material increased. Therefore it can be concluded that the essential oil of Artemisia Argyi from Qichun and the refined moxa wool is basically safe. Involatile substances such as Juniper camphor, Caryophyllene oxide and Caryophyllene etc. are the main contents of high proportional moxa wool of old year. And these substances may be the effective components in moxibustion treatment.

[Fingerprint analysis of Radix Glycyrrhizae by fast HPLC].

The objective of this paper is to develop a fast analysis method to determine fingerprints of Radix Glycyrrhizae from different areas of China for identification and quality control. The experiments were carried out under following conditions: Agilent Eclipse Plus C18 (4.6 mm x 50 mm, 1.8 microm) column, acetonitrile and 0. 05% phosphoric acid solution as the mobile phases with gradient elution, flow rate 1.0 mL x min(-1), analysis time 11 min. The run time of the method was obviously decreased from 36 minutes to 11 minutes compared with routine HPLC method. The cluster analyses of the fingerprints of the 70 samples were performed by SPSS. The results showed that all samples were classified into 2 groups, 59 Glycyrrhiza uralensis as well as 11 G. inflata. Three compounds, liquiritin apioside, liquiritin and glycyrrhiza acid should be considered as effective references for quality control of Radix Glycyrrhizae. This method can be used widely for identification and quality control of Radix Glycyrrhizae.

[Study of quality standards on Qianshan Huoxue plaster].

OBJECTIVE: To establish the methods of identification and assay in Qianshan Huoxue Gao. METHOD: Using TLC to identify Sanchi, Dragon's Blood and using HPLC to determine the content of ginsenoside Rg1. RESULT: The linear range of ginsenoside Rg1 was from 0.153 9 to 1.026 microg. The average recovery was 97.4%, RSD was 2.1%. CONCLUSION: The methods are simple and have good reproducibility.