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OBJECTIVE：To e valuate the correlation between processing time ，color and chemical composition content in the wine-fried process of Salvia miltiorrhiza . METHODS ：Wine-fried S. miltiorrhiza with different processing time （7-15 min）was prepared by yellow rice wine. The contents of salvianolic acid B ，tanshinone ⅡA and 5-HMF in raw and wine-fried S. miltiorrhiza were determined by HPLC. The colorimeter was used to determine their chromatic values [red-green axis component （a*）， yellow-blue axis component （b*），lightness（L*）] and calculate the total color difference value （ΔE）. Spearman ’s rho and Kendall ’s Tau-b test were adopted to validate the correlation between processing time ，chromatic value and chemical composition content. RESULTS：The contents of salvianolic acid B ，tanshinone ⅡA and 5-HMF were 17.9-70.6，2.3-3.1，0 mg/g in S. miltiorrhiza decoction pieces ；the contents of them were 14.8-68.4，1.1-3.9，0.7-34.4 mg/g in wine-fried S. miltiorrhiza . The content of salvianolic acid B at first decreased and then increased ，reaching the peak at about 9，11 min，and then gradually decreased ；the content of tanshinone ⅡA increased at first ，reached its peak about 7 min，and then gradually decreased；the content of 5-HMF increased sharply after frying 13 min. The measurement results of chromaticity values were ΔL* －5.369-2.553，Δa* －1.098-0.321， Δb* －1.471- 2.355，ΔE 0.217-5.397. Results of Spearman ’s rho and Kendall ’s Tau-b test showed that ΔE was positively correlated with processing time （the correlation coefficient were 0.517，0.389 respectively）and 5-HMF content （the correlation coefficient were 0.549，0.405 respectively）（both P＜0.01）. The content of tanshinone ⅡA was negatively correlated with Δb（* the correlation coefficient were －0.509，－0.391 respectively），processing time （the corr elation coefficient were －0.556，－0.420 respectively） and 5-HMF content （the correlation coefficient were －0.545，－0.392 respectively）（both P＜0.01）. The content of 5-HMF was positively correlated with the processing time （the correlation coefficient were 0.957，0.870 respectively）（both P＜0.01）. CONCLUSIONS ：The contents of tanshinone ⅡA and 5-HMF in the process of wine-fried process are significantly related to the time and color. With the increase of processing time and temperature ，its color changes from red 话：0553-3844333。E-mail：liulj1@126.com yellow to yellow green ，and tends to be black in black and white；the content of tanshinone ⅡA is decreased and the content of 5-HMF is increased.
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Objective: To screen the differential ingredients between crude and wine-processed Corni Fructus and determin their content. Methods: An integrated strategy using ultra performance liquid chromatography coupled with tandem quadrupole time-of- flight mass spectrometry (UPLC-Q-TOF/MS) and the chemometric approach was applied to compare the global chemical profile of crude and wine-processed Corni Fructus. Then, the main differential ingredients were quantified by UPLC-PDA. Results: The chemical profiling of wine-processed Corni Fructus was significantly different. Ten compounds could be considered as characteristic chemical markers for distinguishing crude and wine-processed Corni Fructus, including 5-hydroxymethyl furfuraldehyde (5-HMF), gallic acid, protocatechuic acid, morroniside, loganic acid, sweroside, cornin, dihydroquercetin, loganin and cornoside. A new UPLC-PDA quantitative method for analyzing simultaneously the above ten compounds in wine-processed Corni Fructus was established. The results of methodology investigation showed that the ten components were well linear within the investigation range (r ≥ 0.999 7). Compared with the crude Corni Fructus, the content of seven components were increased, including gallic acid, 5-HMF, loganin, morroniside, cornin, sweroside and dihydroquercetin, and the other three components in wine-processed Corni Fructus were decreased. Conclusion: The differential ingredients obtained by chemometric-based approach can be used to distinguish crude and wine-processed Corni Fructus. The determination method of wine-processed Corni Fructus established is accurate and reliable, which can be used for the quality control of Corni Fructus.
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The chromaticity space parameters of the samples during the processing of Gardeniae Fructus Praeparatus(Jiaozhizi in Chinese herbal name, JZZ) were measured by the visual analyzer to analyze the color variation rule during the processing of JZZ, and the content changes of total reducing sugar, total amino acid and 5-hydroxymethylfurfural(5-HMF) related to Maillard reaction were measured. Pearson correlation analysis and linear regression analysis of the data were carried out by SPSS 24.0 software. The experimental results showed that the objective coloration of the samples in the processing of JZZ was basically consistent with the traditional subjective color judgment; the contents of total reducing sugar and total amino acids showed a decreasing trend during the processing of JZZ, and the content of 5-HMF showed an increasing trend, which was in line with Maillard reaction law. Pearson correlation analysis results showed that there was a significant correlation between the chromaticity space parameters L~*(lightness value), a~*(red green value), b~*(yellow blue value), E~*ab(total color value) and the contents of total reducing sugar, total amino acid and 5-HMF(P<0.01), among which the values of L~*, a~*, b~*, E~*ab were positively correlated with the contents of total reducing sugar and total amino acid, and negatively correlated with the contents of 5-HMF. The results of linear regression analysis also showed that these two were highly correlated. In this study, by establishing the correspondence relationship between the color change of JZZ processing and Maillard reactants, wecan not only provide a basis for the objective digital expression of subjective color of JZZ, but also provide a reference for explaining the processing mechanism of JZZ from a new perspective.
Subject(s)
Amino Acids , Color , Drugs, Chinese Herbal , Fruit , Gardenia , Maillard ReactionABSTRACT
Objective: To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid (QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods: YMC ODS column (250 mm × 4.6 mm, 5 μm) was used, column temperature was set at 35 ℃, gradient elution with 0.1% formic acid aqueous solution- acetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was 10 μL. Results: The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08—1.60, 0.12—2.40, 0.09—1.80, 0.06—1.20, 0.10—2.00, 0.30—6.00, 0.01—0.20, 0.01—0.20, 0.01—0.20, 0.005—0.10, 0.005—0.10, and 0.01—0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%, 2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56—102.56, 204.28—212.10, 18.53—18.89, 1.95—2.05, 12.31—12.54, 87.01—87.12, 5.35—5.43, 16.08—16.15, 8.69—8.72, 8.89—8.95, 5.12—5.19, and 1.87—1.94 μg/mL. Conclusion: The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.
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Objective: To explore the potential Q-markers between crude Schisandrae Chinensis Fructus (SCF) and vinegar-processed Schisandrae Chinensis Fructus (VSCF) based on multivariate statistical analysis and network pharmacology. Methods: UPLC-Q/TOF-MS was used to analyze the main lignans in SCF and VSCF, and the potential differences of chemical components (Q-markers) between SCF and VSCF were screened out by using multiple statistical methods. Furthermore, through network pharmacology and bioinformatics, the main action targets and pathways related to significantly different components were analyzed to construct the “component-target-pathway” network relationship and predict the potential quality markers between SCF and VSCF. Results: In this study, 40 different constituents of Schisandra chinensis between SCF and VSCF were screened, among which eight chemical markers had significant differences between SCF and VSCF. Five chemical constituents were identified and confirmed, namely 5-HMF, deoxyschizandrin and its isomer, schisandrin B, and schisantherin D. The other three chemical markers were speculated to be lignans by analyzing the first-and second-order mass spectrometry information. The results of network pharmacological analysis showed that the five potential quality markers identified were highly related to the main pharmacological effects of SCF. Finally, schisandrin B and 5-hydroxymethyl furfural were identified as the most representative potential quality markers. Conclusion: The results showed that the chemical composition of SCF had a series of complex changes. It was determined that schisandrin B and 5-hydroxymethyl furfural could be used as representative potential quality markers between SCF and VSCF. It is speculated that lignans may be the basis of the important effect of VSCF on liver protection.
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Objective: To establish a method of quantitative analysis of multi-components by single marker (QAMS) for medicinal materials and pieces of Cornus officinalis. This method was used in combination with electronic-eye and electronic-tongue technique, and the best steaming time of Cornus officinalis was selected. Methods: Medicinal materials and pieces of C. officinalis were used as the research objects. The contents of five components were determined by establishing the relative correction factor (RCF) of gallic acid, 5-hydroxymethyl furfural (5-HMF), morroniside, cornuside, and internal reference loganin in C. officinalis. Color and taste were measured by electronic eye and electronic tongue technique. The data were analyzed by principal component analysis (PCA), and the best steaming time was optimized by analyzing the results of three methods. Results: The five compounds were well separated. The RSD values of precision and reproducibility were all less than 2%. The stability was good in 24 h. The linear relationship among the concentration and peak areas of the five compounds was all linear (r ≥ 0.999 6). The average recoveries were between 98% and 100.1% and the RSD values were all less than 2%; The RCFs of loganin with the other four compounds were 0.560, 1.344, 1.255, and 0.972 in a linear range. In the principal component analysis (PCA), the sums of main components were 94.618% and 94.98% and the discrimination indexes (DI) were 98 and 93, which indicated that all the samples of C. officinalis could be distinguished well by the electronic-eye and the electronic-tongue. The results showed that the optimum steaming time of C. officinalis was 4 h. Conclusion: The best steaming time of C. officinalis can be optimized by the combination of QAMS with electronic-eye and electronic-tongue techniques.
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Objective: By HPLC, to explore the differences of adjuvants for the changes of chemical components of Rehmanniae Radix Praeparata during process by steamed for nine times and shined for nine times. Methods: HPLC was conducted on a Hypersil GOLD aQ C18 column (250 mm×4.6 mm, 5 μm), flow rate was 1 mL/min, and the column temperature was 25℃. With the mobile phase of acetonitrile and 0.1% phosphoric acid water (1:99), the detection wavelength was 210 nm (catalpol), 203 nm (rehmannioside A, rehmannioside D, and leonuride), acetonitrile and 0.1% phosphoric acid water (3:97 and 4:96); 334 nm (actecosode), acetonitrile and 0.1% phosphoric acid water (16:84), and 284 nm (5-HMF), acetonitrile and 0.1% phosphoric acid water (11:89). Sugars was conducted on an Accurasil NH2 column (250 mm×4.6 mm, 5 μm) with the mobile phase of acetonitrile and 0.1% phosphoric acid water (72:28), flow rate was 1 mL/min, the column temperature was 25℃. The detector was ELSD, Alltech2000ES, drift tube temperature was 93℃, and the gas flow rate was 2.6 L/min. The statistic analysis was carried out by SPSS 20.0 and the paired sample t-test was carried out for 12 kinds of chemical composition in Rehmanniae Radix Praeparata obtained by steamed for nine times and shined for nine times and wine-steamed for nine times and shined for nine times. Results: With the increase of steamed times, the contents of catalpol, leonuride, actecosode, stachyose, sucrose, and raffinose in Rehmanniae Radix Praeparata obtained by two ways are all decreased; While the contents of rehmannioside A and rehmannioside D were slightly increased; the contents of 5-HMF, fructose, glucose, and mannose trisaccharide were increased. Conclusion: The established method conforms to the validation requirement of the methodology. In the process of Rehmanniae Radix Praeparata with steamed for nine times and shined for nine times, processing adjuvant has a marked impact on the quality of the processed product. And the related substances of Rehmanniae Radix Praeparata obtained by the two ways have a larger fluctuation in times 3,4, and 6 of steamed and shined processes, and the reason for this still needs to be further studied.
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Objective:To establish a method for the determination of related substances in enoxacin gluconate injection by HPLC with gradient elution. Methods:HPLC was performed on a DiamonsilTM C18 column (250 mm × 4. 6 mm, 5 μm), the mobile phase A was 0. 025 mol·L-1 phosphonic acid solution (adjusting pH to 3. 0 with triethylamine)-methanol- acetonitrile (80∶10∶10) and the phase B was 0. 025 mol·L-1 phosphonic acid solution (adjusting pH to 3. 0 with triethylamine)-methanol-acetonitrile (350∶325∶325) with gradient elution at a flow rate of 1. 1 ml·min-1 , the detection wavelength was 269 nm and 284 nm, the injection volume was 20μl, and the column temperature was 40℃. Results:Under the HPLC conditions, the samples had good stability and separation. The calibration curve was linear within the concentration range of 19. 80 ng·ml-1-19. 80 μg·ml-1(r=0. 999 9) for 5-hydroxymethylfur-fural with the detection limit of 0. 18ng, and the average recovery was 99. 68% with RSD of 0. 12% (n=9). Conclusion:The method is accurate, sensitive, specific and reproducible, and can be used in the determination of related substances in enoxacin gluconate in-jection.
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Objective:To establish the determination methods for 5-HMF during the processing of polygonatums by HPLC and GC-MS. Methods:The contents of 5-HMF during the processing of three species of polygonatum were determined by HPLC and GC-MS, and the correlation curve of the processing time and the contents was established to study the change regularity of 5-HMF during the processing. Results:The contents of 5-HMF in the three species of polygonatum processed by steamed and stewed methods reached the peak value in 16h or so. The 5-HMF contents in the three species of polygonatum showed significant difference in the order of Polygo-natum cyrtonema Hua>Polygonatum kingianum Coll. et Hemsl. >Polygonatum. sibiricum Red. After the processing, the content of 5-HMF was increased, and the increase in stewed method was more notable than that in steamed method. Conclusion: The study pro-vides theoretical basis for the further study on the processing of polygonatum.
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This study was aimed to analyze the content variations of chemical constituents produced in fresh Radix Rehmanniae (Xian-Di-Huang) after processing into Radix Rehmanniae Recens (Sheng-Di-Huang) and Radix Rehmanniae Preparata (Shu-Di-Huang). HPLC was used in the study of preparing Xian-Di-Huang into Sheng-Di-Huang, and the processing into Shu-Di-Huang. The contents of two newly produced chemical components, which were 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one (DDMP) and 5-hydryoxymethyl-furfural (5-HMF). The contents of both chemical components were determined in Sheng-Di-Huang and Shu-Di-Huang bought from the market. The Zorbax SB-C18 column (250 mm í 4.6 mm, 5 μm) was used. The mobile phase was methanol-wa-ter (5:95). The flow rate was 1.0 mL·min-1. The detection wavelength was set at 280 nm. The results showed that no DDMP or 5-HMF was detected in Xian-Di-Huang. However, after processing, DDMP and 5-HMF can be de-tected in both Sheng-Di-Huang and Shu-Di-Huang. The content in Shu-Di-Huang was higher than that in Sheng-Di-Huang. Both contents in Shu-Di-Huang were gradually increased along with processing time. The con-tent reached to the highest level after processing for 24 h and 32 h, respectively. And then, the content decreased. Both DDMP and 5-HMF were detected from three batches of Sheng-Di-Huang and ten batches of Shu-Di-Huang bought from the market. The content of 5-HMF was higher in Shu-Di-Huang than in Sheng-Di-Huang. There was no obvious difference in the content of DDMP between Sheng-Di-Huang and Shu-Di-Huang. It was concluded that DDMP and 5-HMF were produced in the processing Sheng-Di-Huang and Shu-Di-Huang. The contents were gradually increased along with the prolonging of processing time. There was obvious difference in the content of 5-HMF in Shu-Di-Huang and Sheng-Di-Huang.
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Objective: To isolate the chemical constituents newly produced in processing of Polygonati Rhizoma and to analyze the content changes during its processing. Methods: Two new chemical constituents were isolated from the processed Polygonati Rhizoma by using chemical extraction and identified by LC-MS. Then HPLC analysis was performed to analyze the content changes of the two newly produced constituents in three species of wine-processed Polygonati Rhizoma during different processing periods. The contents of the two compounds in 15 batches of commercially available wine-processed Polygonati Rhizoma were determined. The HPLC was performed on a Zorbax SB-C18 column (250 mm × 4.6 mm, 5 μm) with methanol-water (8:92) as the mobile phase at 1.0 mL/min, detection wavelength was 280 nm, and column temperature at 45°C. Results: The newly produced chemical constituents were 2, 3-dihydro-3, 5-dihydroxy-6-methyl-4H-pyran-4-one (DDMP) and 5-hydryoxymethyl-furfural (5-HMF). The content of DDMP in Polygonatum cyrtonema increased to the top when processed to 24 h and then decreased. The content of 5-HMF was increased gradually throughout the processing. The two chemical constituents were found in the three kinds of wine-processed Polygonati Rhizoma. In the 15 batches of commercially available Polygonati Rhizoma, the range of DDMP in 13 batches was from 1.395% to 5.265%, and the range of 5-HMF in 14 batches was from 0.079% to 0.708%. Moreover, the contents of the two constituents in the three kinds of wine-processed Polygonati Rhizoma (16 h) were within the above ranges. Conclusion: The contents of the two chemical constituents in Polygonati Rhizoma change with the processing time. Therefore, these results could provide the basis for making the quality standard and defining the processing time endpoint of Polygonati Rhizoma.
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Heat induced color change kinetics in a tuna-vegetable mixture was evaluated by measuring color parameter "L" (Hunter-Lab) and 5-hydroxi-methyl-furfural (5-HMF) accumulation. For this purpose small reusable stainless steel TDT cans were used and the kinetic studies performed in a temperature range characteristic of thermal processing of low acid canned foods (110-125°C). The color parameter L was better described by a pseudo zero order while a pseudo first order reaction was found for 5-HMF accumulation, indicating the progression of the Maillard reaction during heating. In both cases, temperature dependence of the rate constants followed the Arrhenius relationship, with Ea= 92.0 and 38.9kJ·mol-1 for lightness L and for 5-HMF accumulation, respectively. The color parameter L was more sensitive to temperature changes than 5-HMF accumulation, and therefore is suggested for evaluation of heat induced color changes in this product.
Se evaluó la cinética del cambio de color inducido por el calor en una mezcla de atún con vegetales mediante la medición del parámetro de color "L" (Hunter-Lab) y la acumulación de 5-hidroxi-metil-furfural (5-HMF). Los estudios cinéticos se llevaron a cabo en un rango de temperatura característico del procesamiento térmico de alimentos de baja acidez (110-125°C), empleando envases TDT reutilizables. El parámetro de color L tuvo un mejor ajuste a una cinética de pseudo orden cero, mientras que la acumulación de 5-HMF se ajustó a una cinética de pseudo orden uno, indicando el desarrollo de la reacción de Maillard durante el calentamiento. En ambos casos, la dependencia de la constante de la velocidad de reacción con la temperatura se ajustó a la ecuación de Arrhenius con Ea= 92,0 y 38,9kJ·mol-1 para la luminosidad L y para la acumulación de 5-HMF, respectivamente. El parámetro de color L fue más sensible a los cambios de temperatura que la acumulación de 5-HMF y por consiguiente se sugiere para la evaluación de los cambios de color inducidos por el calor en este producto.
Foi avaliada a cinética da mudança de cor induzido pelo calor em uma mistura de atum com vegetais mediante a medição do parâmetro de cor "L" (Hunter-Lab) e a acumulação de 5-hidroxi-metil-furfural (5-HMF). Os estudos cinéticos foram levados a efeito em uma faixa de temperatura característica do processamento térmico de alimentos de baixa acidez (110-125°C), empregando envases TDT reutilizáveis. O parâmetro de cor L teve um melhor ajuste a uma cinética de pseudo ordem zero, enquanto que a acumulação de 5-HMF foi ajustada a uma cinética de pseudo ordem um, indicando o desenvolvimento da reação de Maillard durante o aquecimento. Em ambos os casos, a dependência da constante de velocidade de reação com a temperatura foi ajustada à equação de Arrhenius com Ea= 92,0 y 38,9kJ·mol-1 para a luminosidade L e para a acumulação de 5-HMF, respectivamente. O parâmetro de cor L foi mais sensível às mudanças de temperatura que a acumulação de 5-HMF e, por tanto, é sugerido para a avaliação das mudanças de cor induzidas pelo calor em este produto.
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Objective: To establish the determination for 5 HMF in Glucose Injection containing the extract of Radix Salviae Miltiorrhizae. Methods: Using HPLC with Hypersil ODS [4.6mm(i.d)?250mm] column, methanol 0.5% acetic acid as a mobile phase and detection wavelength at 284nm. Results: The peak of 5 hydroxymethylfurfural was separated from the peak of Danshensu. Conclusion: The method is simple, sensitive and accurate with a good reproducibility and can be used as the quality control for Glucose Injection containing the extract of Radix Salviae Miltiorrhizae.