Qualitative and quantitative analysis of major components of Qiye Shen'an tablet by UPLC Q-TOF/MS and UPLC-TQS-MS/MS.

The Qiye Shen'an tablet is formulated using total saponins extracted from Notoginseng stems and leaves. At present, the study on its chemical composition remains scarce and the quality control indicators are limited, which seriously hindering the effective quality control and clinical research. Hence, this study aims to comprehensively identify and characterize the Qiye Shen'an tablet while controlling its main component contents. To achieve a comprehensive understanding of this tablet, an ultra-high performance liquid coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS) method was employed for its separation and characterization. Through the analysis of 99 batches of Qiye Shen'an tablet produced by 9 enterprises, the characteristic quantitative components were further obtained. A total of 113 compounds were characterized and identified, among which 17 representative compounds were selected, and the ultra-high performance liquid-triple quadrupole tandem mass spectrometry (UPLC-TQS-MS/MS) method was established for further quantitative determination. It has been successfully applied to the content determination of 99 batches of Qiye Shen'an tablet, and a new quality control method is being formed. This study provides a new method for chemical spectrum analysis and determination of labeled compounds of Qiye Shen'an tablet, and lays a solid foundation for further study of potential active ingredients and comprehensive quality evaluation.

Quantification and holistic quality evaluation of Wulingzhi extract by UHPLC-Q-Orbitrap-HRMS coupled with chemometric approaches.

The excreta of Trogopterus xanthipes ("Wulingzhi" in Chinese, WLZ) is a well-known traditional Chinese medicine. It has been used for centuries to treat amenorrhea, menstruation and postpartum abdominal pain. However, a systematic quality study on WLZ chemical markers has yet to be conducted. This study aimed to establish an ultra-high-performance liquid chromatography coupled with a hybrid quadruple extraction Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap-HRMS) method for the simultaneous quantitative determination of 20 compounds in 53 batches of WLZ; the method rapidly and sensitively determined the 20 plant- or animal-derived compounds. Firstly, the proposed approach was validated to satisfy the method's linearity, detection limits, precision, repeatability, stability and accuracy. Subsequently, multivariate analysis was used to identify correlations between the samples and feed, processing and regions. Finally, this method was used to further identify chemical markers for quality control in combination with chemometrics. This is the first report on pinusolide, betaine, hippuric acid, 4-oxorentinoic acid, 15-methoxypinusolidic acid and 4-oxoisotrentinoin in WLZ; the quality of WLZ became homogeneous after processing with vinegar (V-WLZ). Moreover, we screened for potential component markers, including uridine, allantoin, amentoflavone, hippuric acid, 3,4-dihydroxybenzoic acid, pinusolide, quercetin and kaempferol. These results were practical and efficient for the chemical clarification of WLZ and V-WLZ.

Impact of rapid rehabilitation surgery on perioperative nursing in patients undergoing cardiac surgery: A meta-analysis.

OBJECTIVE: To systematically evaluate the effect of enhanced recovery after surgery (ERAS) on perioperative nursing of patients undergoing cardiac surgery. METHODS: A systematic literature search was performed in PubMed, Embase, Web of science, Cochrane, CNKI, Wanfang, and VIP using predefined search strings from inception of database to May 2021. Randomized control trials (RCTs) with sample size >40 on cardiac surgery with either ERAS nursing or routine nursing reporting extubation (trachea) time, length of stay, out of bed activity time, and nursing satisfaction were included in the analysis. Stata SE 12.0 software was used for statistical analysis. RESULTS: A total of 27 RCTs were included. All the included studies were Chinese due to lack of studies in English. The results of meta-analysis showed that the extubation time standardized mean difference ([SMD] = -3.11; 95% confidence interval [CI]: -3.77, -2.45; p < .001), out of bed activity time (SMD = -2.89; 95% CI: -3.34, -2.44; p < .001), and hospitalization time (SMD = -2.08; 95% CI: -2.37, -1.79; p < .001) of cardiac surgery patients with ERAS nursing was significantly shorter than those with routine nursing. The patient's satisfaction after surgery with ERAS was higher than that of routine nursing relative risk ([RR] = 1.24; 95% CI: 1.18, 1.30; p < .001). CONCLUSION: ERAS nursing can accelerate perioperative rehabilitation of patients undergoing cardiac surgery and highly accepted by patients.

[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 Prostaglandin and Hormones in Excreta of Trogopterus xanthipes.

The excreta of Trogopterus xanthipes (also called Wulingzhi in Chinese, WLZ) is a well-known traditional Chinese medicine used for the treatment of irregular menstruation in clinic. Few reports are available on the chemical profiling of WLZ. In this work, qualitative and quantitative analyses of endogenous prostaglandin and hormones in WLZ were performed using UHPLC-orbitrap-MSn. In total, 48 compounds were identified in urine of T. xanthipes. Furthermore, the contents of four target compounds were simultaneously quantitated in 20 batches of samples by UPLC-MS/MS. The quantitative method showed a good linear correlation (R > 0.995) in a wide range for each compound. The method had a high sensitivity with LOD (0.5-1.0 ng/mL) and LOQ (1.0-2.5 ng/mL). The intra- and inter-day precisions were < 9.17 (RSD %), and repeatability and stability were < 6.14 (RSD %). The recovery of the analytes varied between 85.8% and 97.3% at three different concentrations. The present integrated qualitative and quantitative assessment of WLZ provides an evaluation strategy to assess the constituent in traditional Chinese medicine.

[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.

[Determination of main free amino acids in Banlangen Keli by UPLC].

OBJECTIVE: To establish a quantitative method with precolumn derivatization for determining the contents of six common amino acids in Banlangen Keli by UPLC. METHOD: Using 6-acetamido-4-hydroxy-2-methyl quinoline as the derivating agent, we determined the contents of arginine, threonine , alanine, gamma aminobutyric acid, proline, and valine. The UPLC analysis was performed on a Waters AccQ Tag TM Ultra C18 column (2.1 mm x 100 mm, 5 microm) with mobile phase AccQ Tag Ultra Eluent A and AccQ Tag Ultra Eluent B gradient elution at a flow rate of 0.7 mL x min(-1). The column temperature was 55 degrees C and detection wavelength was 260 nm. RESULT: The linear ranges of arginine, thremine, alanine, gamma aminobutyric acid, proline, and valine were 4. 15549.86 microg (r = 0.999 9), 0.595-5.95 microg (r = 0.999 8), 0.445-4.45 microg (r = 0. 999 9), 0.515-5. 15 pg (r = 0.999 9), 8.858-106.3 microg (r = 0.999 9) , 0.585-5. 85 microg (r = 0.999 8). Their average recoveries were 100.6%, 98.35%, 100.2%, 98.44%, 98.34%, 98.18% with RSD 1.8%,1.9%, 2.0%, 2.4%, 1.5% and 2.0%, respectively (n = 6). The contents of amino acids were different in samples from five productive enterprises. CONCLUSION: The method is efficient, good reproducible, sensitive, and accurate.

[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.