Research on relationship between color and composition changes in processing of rhubarb charcoal based on "external and internal correlation" / 中草药

Objective: To study the relationship between the quantitative color value of the powder and the known component content of rhubarb charcoal, and lay the foundation for the establishment of the rhubarb charcoal processing process control and endpoint judgment based on the color quantitative value. Methods： Rhubarb charcoal samples were prepared at different temperatures and time. Based on the empirical judgment of the rhubarb charcoal processing, the visual analyzer and UV-Vis were used to quantify the color of the pieces and powder of rhubarb charcoal under different processing conditions. At the same time, the HPLC fingerprint method was used to evaluate the dynamic changes of chemical components during the processing of rhubarb charcoal, and the quantitative value of the color of the sample during the processing of rhubarb charcoal was correlated with the characteristic components of the HPLC fingerprint using the multivariate statistical method. Results: During the processing of rhubarb charcoal, as the degree of carbonization increased, the apparent color of the sample changed from light yellowish brown to burnt black. There was a high correlation between the lightness value (L*), red-green value (a*) of the sample pieces and powder and the yellow and blue values (b*). The area of the 26 characteristic peaks had varying degrees of correlation with the chromaticity value. Among the 14 known components, five bound anthraquinones (aloe-emodin-8-O-β-D-glucoside, rhein-8-O-β-D-glucoside, chrysophanol-8-O-β-D- glucoside, emodin-8-O-β-D-glucoside, physcion-8-O-β-D-glucoside), and two sennosides (sennoside A, sennoside B) had a linear positive correlation with the chromaticity value. The content of five free anthraquinones (aloe-emodin, rhein, chrysophanol, emodin, and physcion), gallic acid and 5-hydroxymethylfurfural (5-HMF), whose contents increased first and then decreased, showed a quadratic correlation with the chromaticity value. Conclusion: The subjective judgment of rhubarb charcoal in the processing process is consistent with the quantitative color value analysis. The quantitative color value has a clear correlation with the content of 14 active chemical components. It is preliminarily inferred that the color quantitative value can be used as the quality of the rhubarb charcoal processing process control and end-point determination indicators to achieve efficient and rapid identification of the processing quality of rhubarb charcoal, which can provide new ideas for the monitoring and quality control of the rhubarb charcoal processing process.

Contents Changes of Polysaccharide and 5-HMF in Polygonati Rhizoma from Different Producing Areas af-ter Different Processing / 中国药房

OBJECTIVE:To study the contents changes of polysaccharide and 5-HMF in Polygonati rhizoma from different pro-ducing areas after different processing,and provide reference for the development of processing technology of Polygonati rhizoma from different producing areas and the quality standard of different processing products. METHODS:UV spectrophotometry and HPLC were conducted to respectively determine the contents of polysaccharide and 5-HMF,and compare the content differences of polysaccharide and 5-HMF in Polygonati rhizoma from different producing areas [Shaanxi Lueyang County,Shaanxi Huangling County,Yunnan Fumin County (genuine producing areas),Shaanxi Taibai County] by fresh-cutting,dry-cutting,steaming and steaming with wine. RESULTS:Polysaccharide of sample from Yunnan Fumin County showed the highest content in fresh-cut sam-ples(13.4%),no 5-HMF(0)was detected;polysaccharide contents were respectively 10.8%-13.4%,8.9%-10.8%,5.5%-6.9%, 5.6%-6.5% after fresh-cut,dry-cut,steamed and steamed with wine,5-HMF contents were 0,0,0.21%-0.50%,0.25%-0.72%. Compared with no processing samples (fresh-cut),polysaccharide contents in Polygonati rhizoma were decreased in turn after dry-cut,steamed and steamed with wine,5-HMF contents were increased in turn after steamed and steamed with wine. CONCLU-SIONS:It is suggested to consider origin factor in developing processing technology of Polygonati rhizoma from genuine and non-genuine producing areas. 5-HMF content determination index should be added into quality standard of processing products after steamed and steamed with wine.

Content of polysaccharide and 5-hydroxymethyl furfural (5-HMF) in Codonopsis Radix after cooked with rice and its impact on rabbit gastrointestinal smooth muscle in vitro / 中草药

Objective: The effect of Codonopsis Radix was significantly different before and after being cooked, and to study the content of polysaccharide and 5-hydroxymethyl furfural (5-HMF) in Codonopsis Radix after cooked with rice and its impact on rabbit gastrointestinal smooth muscle in vitro. Methods: Before and after being cooked, the content of polysaccharide and 5-HMF were determined with phenol sulfuric method and HPLC. BL-420F bio-functional experiment was applied to observe the impact of Codonopsis Radix processing with rice on rabbit gastrointestinal smooth muscle in vitro. Tests showed that acetylcholine (Ach), neostigmine, barium chloride (BaCl2), atropine, and adrenaline (Adr) intervened the relaxation of rabbit gastrointestinal smooth muscle in vitro. Results: The content of polysaccharide was significantly lower than pieces after cooked with rice, and the content of 5-HMF was significantly higher. After processing it can further excite spontaneous activity of gastrointestinal smooth muscle in vitro. It can enhance bowel neostigmine and BaCI2 caused intestinal excitement and tension, objecting Adr caused intestinal relaxation. Conclusion: 5-HMF was abundantly produced after Codonopsis Radix cooked with rice, caused excitability contraction on rabbit gastrointestinal smooth muscle in vitro, reproducing 5-HMF effect of gastrointestinal smooth muscle in vitro. It may be one of the material basis of Codonopsis Radix cooked with rice enhanced spleen. Its mechanism may be its collaborative control of N2R and βR results.

Maillard Reaction Products in Powder Based Food for Infants and Toddlers.

Aim: To investigate the formation of Maillard reaction products (MRPs) during 28 days storage of the two most consumed brands (B1, B2) of gruel products on the Swedish market. Methodology: The MRPs; furfural, 5-hydroxymethyl furfural (HMF), N-(1-Carboxyethyl)-L-Lysine (CEL), N-(1-Carboxymethyl)-L-Lysine (CML), fluorescent advanced glycation end products (AGEs) and melanoidins (brown colour) were selected for analysis. High performance liquid chromatography coupled to UV spectrophotometry, fluorescence spectrophotometry or tandem mass spectrometry was used for analysis. Results: In general, MRPs were higher in B2 than in B1 at the time of opening the package. The initial content of MRPs in B1 and B2 respectively was as follows: 4.39 and 13.74 μg/g of furfural; 1.11 and 1.47 μg/g of HMF; 73.64 and 134.3 μg/g of total CML; 19.79 and 30.42 μg/g of total CEL; 51.11 and 73.01 AU/g of fluorescent AGEs; 0.52 and 1.45 AU/g of MRPs that absorb light at 420 nm and 1.40 and 3.22 AU/g of MRPs that absorb light at 360 nm. During storage for 28 days, furfural, HMF, MRPs that absorb light at 360 nm and at 420 nm as well as fluorescent MRPs increased significantly by respectively 7, 30, 60, 83 and 21% in B2. In B1, only the fluorescent MRPs (21%) increased during storage. Conclusion: A higher initial content and more pronounced increase of MRPs during 28 days storage time was observed in B2. Consequently, children consuming gruel from B2 are exposed to 1.3-3.1 times more MRPs compared to B1. Considering that a child often sticks to one gruel brand throughout the first years of life and that some MRPs are inflammatory drivers, more studies are required to understand the role of food-process induced chemicals at an early age for future health of the children.

Improvement of extraction and concentration on quality consistency of Qiongyu Paste / 中草药

Objective: To explore the influence of extraction and concentration with long duration on the quality consistency of Qiongyu Paste (QYP), and to analyse the degradation and transformation mechanisms of each component involved in the quality change of QYP. Methods: QYP was a paste formula derived from Rehmanniae Radix, Poria, and Ginseng Radix et Rhizoma in a weight ratio of 7∶2∶1, the contents of 10 major bioactive components [5-hydroxymethyl furfural (5-HMF), catalpol, melittoside, acetoside, ginsenoside Re, ginsenoside Rb1, ginsenoside 20(S)-Rg3, ginsenoside Rg1, ginsenoside Ro, and pachymic acid] were simultaneously determined by the previously established HPLC-MS method. The standard deviation (SD) accumulation values of the contents of 10 bioactive components in repeatedly prepared samples in different durations were compared. Results: Total contents of the 10 components and relative contents of some individual components in QYP changed significantly with different extraction and concentration duration. At the same time, the SD values of the contents of bioactive components in repeatedly prepared samples decreased with extending the extraction and concentration duration. Conclusion: Extraction and concentration could improve the quality consistency of QYP.

Optimization of Processing Technology of Nine Steaming Nine Drying of Rehmannia glutinosa by Multiple Indexes Comprehensive Balance Method-Orthogonal Test / 中国药房

OBJECTIVE:To optimize the processing technology of nine steaming nine drying of Rehmannia glutinosa. METH-ODS:L9(34) orthogonal experimental design was adopted to investigate the effects of the amount of added wine,steaming time and drying way on processing technology using the content and property of 5-hydroxymethyl furfural,acteoside,reducing sugar wa-ter extract,and character score as indexes. Comprehensive balance method was used for result evaluation,and optimized technolo-gy was validated. RESULTS:The optimized processing condition was as follows as the amount of added yellow wine 40%,steam-ing for 9 times,lasting for 6 h each time,blast drying at 70 ℃. Average value of each factor in validation test was 4.030 mg/g, 0.117 mg/g,0.376 7 g/g,0.733 g/g and 9.0 points,respectively. Their RSDs were 1.78%,2.9%,1.54%,2.13% and 0.1%(n=3). CONCLUSIONS:Optimized technology is reasonable and controllable in product quality,and can provide reference for quality control study of nine steaming nine drying of R. glutinosa.

Quality analysis of Liuwei Dihuang Concentrated Pills based on multi-index components / 中草药

Objective: To establish a determination method for the simultaneous determination of the multiple components in Liuwei Dihuang Concentrated Pills (LDCP). Methods: The contents of gallic acid, 5-hydroxymethyl furfural, morroniside, loganin, paeoniflorin, paeonol, and ursolic acid were used as observing indexes. HPLC method, Agilent TC-C18 (250 mm × 4.6 mm, 5 μm) column using acetonitrile-0.02% TFA as mobile phase, gradient elution volume flow was 1.0 mL/min, column temperature was 30℃; Detection wavelengths were 0-60 min, 238 nm, 60-70 min, and 210 nm; Cluster analysis method was used to compare the differences of LDCP among 20 different manufacturers. Results: The seven ingredients in LDCP from different manufacturers were determined. There was difference among them, the contents of paeoniflorin showed appreciable difference. The products from 20 manufacturers were divided into two categories by the cluster analysis, and showed obvious difference between them. The numbers 4, 6, 8, 9, 11, 14 and 16 were classified into one group, which quality difference was relatively minor; The products from other manufacturers belonged to one category and there were little differences among the seven components. Conclusion: The methodology research shows that this methed could fit the demand of determination and provides some guidance to advance the quality evaluation of LDCP.

Chemical constituents from rhizomes of Valeriana jatamansi / 中草药

Objective: To investigate the chemical constituents from the rhizomes of Valeriana jatamansi. Methods: The ethanol percolation extraction was isolated and purified by ODS column, silica gel column, and Sephadex LH-20 chromatography. All compounds were identified on the basis of spectral analysis. Results: Thirteen compounds were isolated from the rhizomes of V. jatamansi and identified as prinsepoil (1), 8-hydroxypinoresinol (2), pinoresinol (3), 2,5-Methanocyclopenta-1,3-dioxin-7-ol (4), 3-(4-hydroxy-3-methoxyphenyl)-propenal (5), vibutinal (6), baldrinal (7), 11-ethoxyviburtinal (8), 5-hydroxymethyl furfural (9), pinoresinol-4'-O-β-D-glucoside (10), (7S,8R)-dehydroconiferyl alcohol-8,5'-dehydroconiferyl aldehyde-4-O-β-D-glucopyranoside (11), magnolol (12), and daucosterol (13). Conclusion: Compounds 11 and 12 are isolated from the plants in Valerianaceae for the first time, compounds 5 and 6 are isolated from the plants of Valeriana L. for the first time, and compounds 9 and 10 are isolated from this plant for the first time.

Chemical constituents in chloroform extraction of Tetrastigmatis hemsleyani diels et Gilg and their antitumor activities / 中国药学杂志

OBJECTIVE: To investigate the chemical constituents in chloroform extraction of Tetrastigmatis hemsleyani diels et. Gilg and their antitumor activities. METHODS: Various chromatography techniques such as column chromatography on silica gel, Sephadex LH-20 and preparative TLC were used to isolate and purify the compounds. Their structures were identified by 1H-NMR, 13C-NMR and MS. Their antitumor activities was tested by MTT method. Moreover, the other compounds of chloroform extraction were detected by GC-MS. RESULTS: Six compounds were isolated by classic chromatography and identified as β-sitosterol(1), 4-hydrox-y-3-methoxybenzaldehyde(2), oleanolic acid (3), 5-hydroxymethyl furfural(4), azelaic acid(5), vanillic acid(6). Twenty-two compounds were identified by GC-MS. CONCLUSION: Compounds 2-6 are isolated from this plant for the first time. Compounds 1 and 3 shows strong cytotoxic activities against Hela229 with IC50 values of 40.78, 25.69 μg · mL-1, respectively. Compound 3 also showed strong cytotoxic activities against with IC50 values of 69.87 μg · mL-1. The result proved that antitumor activity of chloroform extraction of Tetrastigmatis hemsleyani diels et. Gilg is due to the contribution of multi-components.

Multiple fingerprints and multi-comonent quantitative analysis of Danhong Injection / 中草药

Objective: To establish the multiple fingerprints of Danhong Injection (DI) using HPLC-UV-MS method and to simultaneously determine nine kinds of the medicinal components in DI. Methods: Separation was performed on Atiantis T3 analytical column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.05% formic acid-50% acetonitrile by gradient elution, and negative-ion SIM mode was selected for mass spectrometric detection. Results: The multiple fingerprints reflected the chemical information of Salvia miltiorrhiza and safflower in DI. The similarity of the fingerprints was higher than 0.988 in all 11 batches of DI. 5-Hydroxymethyl furfural, sodium danshensu, protocatechuic aldehyde, coumaric acid, salvianolic acid D, rosmarinic acid, salvianolic acid B, salvianolic acid A, and kaempferol-3-O-rutinoside showed the good linearity in their respective ranges of concentration, r ≥ 0.999 0.The average recovery of low-, mid-, and high-dose medicinal components (n = 9) was (99.0 ± 1.4)%, (102.0 ± 1.7)%, (99.3 ± 1.6)%, (97.6 ± 1.6)%, (100.0 ± 1.8)%, (97.9 ± 1.6)%, (100.5 ± 4.4)%, (100.6 ± 2.0)%, and (106.0 ± 4.7)%, respectively. The relative standard deviation for the method reproducibility was lower than 1.45%. The total contents of nine medicinal components in the 11 batches of DI were 2.61-3.06 mg/mL. Conclusion: This method is simple, accurate, and with good reproducibility, and the multiple fingerprints combined with the quantitative analysis could reflect the quality of DI better, which could be used to control the quality of DI.

Simultaneous quantitation of four antioxidant components in Alpinia oxyphylla Miq. by UPLC / 中国药学杂志

OBJECTIVE: To establish a UPLC method for simultaneous determination of 5-hydroxymethyl furfural (1), leu-hetenone A (2), lectochrysin (3), and nootkatone (4) in Alpinia, oxyphylla Miq, and to compare the contents of the four components in different parts of this medicinal materials from different places. METHODS: The UPLC method was established on an HSS T3 Column (2.1 mm × 100 mm, 1.8 μm). The mobile phase consisted of water containing 0.1% formic acid and acetonilrile in gradient elution mode at the flow rate of 0.5 mL · min-1 and the detection wavelength was set at 255 nm. RESULTS: The standard curves of compounds 1, 2, 3, and 4 showed good linearity in the ranges of 1.223-24.46, 2.016-40.32, 1.875-37.50 and 16.78-335.6 μg · mL-1 with the corresponding average recoveries of 99.5%, 101.5%, 100.9% and 101.2%, respectively. CONCLUSION: The method is precise and highly reproducible, which can be used to simultaneously determine the antioxidant components including 5-hydroxymelhyl furfural, teuhetenone A, tectochrysin, and nootkatone in Alpinia oxyphylla Miq; compounds 2 and 4 are mainly extracted from the seeds, while compounds 1 and 3 come from the seeds and putamens equally. There are significant differences among the samples from different production areas.

TLC for Distinguishing the Crude and Processed Radix of Polygonum Multiflorum Thunb / 中国中医药信息杂志

Objective To study the method for distinguishing the crude and processed Radix of Polygonum multiflorum Thunb. by TLC. Methods Some of the samples were collected from different cities in China, some of them were prepared following the pharmacopoeia standard or local standard. TLC conditions: 5-hydroxymethyl-furfural (5-HMF) was used as a standard matter with the developing solvent of petroleum ether (60～90 ℃)-ethyl acetate (1∶1) on a silica G thin layer plate, sprayed with 15% ?-naphthol in ethanol solvent, heated and detected in daylight. Results TLC chromatogram showed that crude and processed product of Polygonum multiflorum Thunb. were different. Conclusion TLC method for distinguishing the crude and processed Polygonum multiflorum Thunb. was established.

Comparison of catalpol and 5-hydroxymethyl-furfural in Radix Rehmanniae at different processing times / 中华中医药杂志

Objective:To approach the determination method of 5-hydroxymethyl-furfural in Radix Rehmanniae,and to investigate influence of steam processing on catalpol and 5-hydroxymethyl-furfural. Methods:Catalpol and 5-hydroxymethyl-furfural from Radix Rehmanniae at different processing time was determined by high performance liquid chromatography. Results:In the steam processing,content of 5-hydroxymethyl-furfural increased with the increase of time in the beginning,when steamed to 52h,the levels began to decline; content of catalpol reduced with increase of the processing time. Conclusion:Content of catalpol and 5-hydroxymethyl-furfural changed signifi cantly in the steam processing.

Contnet Determination of 5-hydroxymethyl Furfural in Rhizoma Rehamanniae Praeparatae by TLC-Scanning Method / 中成药

The stable brownish red phenylhydrazone compound formed by the combination of 5-hy- droxymethyl furfural with 2,4-dinitrophenylhydrazine showed the maximum absorption at 493nm wavelength of chromatic spectrum.So 5-hydroxymethyl furfural content can be deter- mined with dual wavelength TLC-scanning method.This method is simple,quick and accu- rate.