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ObjectiveTo discriminate the age of Arisaema Cum Bile, the combination of headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was applied to explore the differences of volatile components of unfermented, 1-year fermented, 2-year fermented, and 3-year fermented Arisaema Cum Bile. MethodSamples with different fermentation durations were collected and HS-SPME-GC-MS technology was employed to detect the volatile components of each sample. The relative contents of detected volatile components were processed and analyzed by chemometrics methods such as principal component analysis (PCA), hierarchical cluster analysis (HCA), and partial least squares discriminant analysis (PLS-DA). ResultThe results showed that 145 volatile components were identified. Among these volatile components, the relative contents of heterocyclic, alcohols, aldehydes and aromatics were high. PCA, HCA, and PLS-DA can effectively separate Arisaema Cum Bile with four different ages. Based on variable importance in projection (VIP) value > 1, 73 markers of differential volatile components were identified. The content of 2,6,11-trimethyldodecane and m-xylene in unfermented samples was the highest, and the content difference between them and those in fermented samples was significant (P<0.05). 2,3-butanediol was detected only in 1-year samples, octane was detected only in 2-year samples, and ethyl heptanoate was detected only in 3-year samples. These components can be used as odor markers for Arisaema Cum Bile with different fermentation years. ConclusionThe identification method of volatile components of Arisaema Cum Bile was established by HS-SPME-GC-MS technology, which can realize the rapid identification of unfermented, 1-year fermented, 2-year fermented, and 3-year fermented samples, and provide a scientific basis for the standardization of processing technology and quality standards of Arisaema Cum Bile.
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ObjectiveTo screen the differential markers by analyzing volatile components in Dalbergia odorifera and its counterfeits, in order to provide reference for authentication of D. odorifera. MethodThe volatile components in D. odorifera and its counterfeits were detected by headspace gas chromatography-mass spectrometry(HS-GC-MS), and the GC conditions were heated by procedure(the initial temperature of the column was 50 ℃, the retention time was 1 min, and then the temperature was raised to 300 ℃ at 10 ℃ for 10 min), the carrier gas was helium, and the flow rate was 1.0 mL·min-1, the split ratio was 10∶1, and the injection volume was 1 mL. The MS conditions used electron bombardment ionization(EI) with the scanning range of m/z 35-550. The compound species were identified by database matching, the relative content of each component was calculated by the peak area normalization method, and principal component analysis(PCA), orthogonal partial least squares-discrimination analysis(OPLS-DA) and cluster analysis were performed on the detection results by SIMCA 14.1 software, and the differential components of D. odorifera and its counterfeits were screened out according to the variable importance in the projection(VIP) value>2 and P<0.05. ResultA total of 26, 17, 8, 22, 24 and 7 volatile components were identified from D. odorifera, D. bariensis, D. latifolia, D. benthamii, D. pinnata and D. cochinchinensis, respectively. Among them, there were 11 unique volatile components of D. odorifera, 6 unique volatile components of D. bariensis, 3 unique volatile components of D. latifolia, 6 unique volatile components of D. benthamii, 8 unique volatile components of D. pinnata, 4 unique volatile components of D. cochinchinensis. The PCA results showed that, except for D. latifolia and D. cochinchinensis, which could not be clearly distinguished, D. odorifera and other counterfeits could be distributed in a certain area, respectively. The OPLS-DA results showed that D. odorifera and its five counterfeits were clustered into one group each, indicating significant differences in volatile components between D. odorifera and its counterfeits. Finally, a total of 31 differential markers of volatile components between D. odoriferae and its counterfeits were screened. ConclusionHS-GC-MS combined with SIMCA 14.1 software can systematically elucidate the volatile differential components between D. odorifera and its counterfeits, which is suitable for rapid identification of them.
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ObjectiveThis study aims to investigate the changes in fungal community diversity and volatile components during the aging process of Aquilariae Lignum Resinatum and explore the internal relationship between them. MethodAquilariae Lignum Resinatum samples with different aging years were collected. High-throughput sequencing was employed to analyze the fungal diversity and abundance, and α and β diversity indicators were calculated to reveal the composition and dynamic changes of the fungal community. In addition, the essential oils of Aquilariae Lignum Resinatum with different aging years were extracted, separated, and identified by two-dimensional gas chromatography-high resolution time-of-flight mass spectrometry. ResultA total of 61 compounds were identified from the volatile components of five groups of Aquilariae Lignum Resinatum samples, including 2 monoterpenes, 24 sesquiterpenoids, 1 diterpene, 13 aromatic hydrocarbons, 9 alkanes, and 12 other compounds. Among them, the volatile compounds isolated from the sample aged for 1 year had the largest number, and those from the sample aged for 2 years accounted for the largest proportion of the total components. The internal transcribed spacer(ITS) amplicon sequencing revealed that the fungi in the five groups of samples belonged to 162 genera. Kirschsteiniothelia, Aspergillus, Lasiodiplodia, Phaeoacremonium, and Trichoderma were the dominant fungal genera. The fungal diversity in the Aquilariae Lignum Resinatum sample aged for 4 years was significantly higher than that in the samples aged for 0 to 3 years. ConclusionThe volatile component content and composition of Aquilariae Lignum Resinatum altered dramatically during aging. The aging of Aquilariae Lignum Resinatum was accompanied by the increasing fungal diversity, decreasing relative content of aromatic hydrocarbons, and increasing relative content of sesquiterpenoids. In general, aging was beneficial to the transformation of sesquiterpenoids and the enrichment of fungi.
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ObjectiveBy comparing the differences in composition and content of volatile components between Atractylodis Macrocephalae Rhizoma(AMR)and bleaching AMR, bran-fried AMR and bran-fried bleaching AMR, the effect of processing with rice-washed water on the volatile components in AMR and bran-fried AMR were investigated. MethodHeadspace gas chromatography-mass spectrometry(HS-GC-MS)was used to determine the volatile components in raw products, bran-fried products and their processed products with rice-washed water. GC conditions were programmed temperature(starting temperature of 50 ℃, rising to 140 ℃ at 10 ℃·min-1, maintained for 5 min, then rising to 210 ℃ at 4 ℃·min-1), splitting ratio of 10∶1, high purity helium as the carrier gas and a solvent delay time of 3 min. MS conditions were an electron bombardment ion source(EI) with an electron collision energy of 70 eV, ion source temperature of 230 ℃, and the detection range of m/z 20-650. The relative contents of the components were determined by the peak area normalization method, the obtained sample data were subjected to principal component analysis(PCA) and orthogonal partial least squares-discriminant analysis(OPLS-DA) by SIMCA 14.1 software, and the differential components of AMR and bleaching AMR, and bran-fried AMR and bran-fried bleaching AMR were screened according to variable importance in the projection(VIP) value>1 and P<0.05. ResultA total of 71 volatile components were identified, including 53 in AMR, 50 in bleaching AMR, 51 in bran-fried AMR, and 44 in bran-fried bleaching AMR. OPLS-DA results showed that there were significant differences between AMR and bleaching AMR, bran-fried AMR and bran-fried bleaching AMR, but not between AMR samples from different origins. The compound composition of AMR and bleaching AMR, bran-fried AMR and bran-fried bleaching AMR did not change, but the contents of monoterpenes and sesquiterpenes changed significantly. ConclusionSignificant changes in the contents of volatile components were observed in AMR and bleaching AMR, bran-fried AMR and bran-fried bleaching AMR, among them, 1,2-dimethyl-4-methylidenecyclopentene, 9,10-dehydro-isolongifolene, γ-elemene, zingiberene, atractylone, silphinene, modhephene and (1S,4S,4aS)-1-isopropyl-4,7-dimethyl-1,2,3,4,4a,5-hexahydronaphthalene can be used as candidate differential markers of volatile components of AMR before and after processing with rice-washed water.
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ObjectiveBy exploring the volatile components, polysaccharide composition and changes in the contents of five carbohydrate components of Polygonatum cyrtonema rhizoma before and after processing, and then the effect of yellow rice wine on the odour formation of P. cyrtonema rhizoma was investigated. MethodThe volatile components of P. cyrtonema rhizoma before and after processing were detected by headspace gas chromatography-mass spectrometry(HS-GC-MS), and sample data were subjected to principal component analysis(PCA) and orthogonal partial least squares-discriminant analysis(OPLS-DA) using SIMCA 14.1, then the differences between these components of P. cyrtonema rhizoma before and after processing were screened according to the principle of variable importance in the projection(VIP) value>1. Crude carbohydrate components in raw and wine-processed P. cyrtonema rhizoma were subjected to oxime and silylation, the carbohydrate components were analyzed by gas chromatography-mass spectrometry(GC-MS/MS), and the relative contents of various components were calculated by peak area normalization, then quantitative analysis of four carbohydrate components was also carried out. ResultA total of 23 volatile components were identified from the raw products and the wine-processed products, including 15 components in raw products and 20 components in wine-processed products. Among them, 2-methylbutyraldehyde and isovaleraldehyde had a sweet odor and their contents increased after processing, but the contents of hexanal and caproic acid decreased, new components such as 2-acetylfuran and 5-methylfuranal were produced after processing. PCA and OPLS-DA results showed that there were significant differences between raw products and the wine-processed products, a total of 13 differential compounds were screened out, of which 7 showed an upward trend in relative content and 6 showed a downward trend. A total of 7 carbohydrate components, including 5 monosaccharides and 2 disaccharides, were identified in raw products and the wine-processed products. The results of determination showed that the contents of fructose, glucose, mannose and sucrose in P. cyrtonema rhizoma increased after wine-processing, and their increases were 4.54, 1.51, 2.93, 3.66 times, respectively. ConclusionAfter processing, the increase of aromatic flavor of P. cyrtonema rhizoma may be related to the increase of the contents of aldehydes such as 2-methylbutyraldehyde and isovaleraldehyde, while the decrease of raw flavor may be related to the decrease of the contents of volatile components such as hexanal and hexanoic acid, the increase of sweet flavor may be related to the increase of the contents of monosaccharides and oligosaccharides such as fructose and sucrose.
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This study aims to compare the chemical constituents in 24 batches of Artemisiae Argyi Folium samples collected from three different Dao-di producing areas(Anguo in Hebei, Nanyang in Henan, and Qichun in Hubei). An ultra-performance liquid chromatography(UPLC) method was established to determine the content of 13 nonvolatile components, and headspace-gas chromatography-mass spectrometry(HS-GC-MS) was employed for qualitative analysis and comparison of the volatile components. The content of phenolic acids in Artemisiae Argyi Folium was higher than that of flavonoids, and the content of nonvolatile components showed no significant differences among the samples from the three Dao-di producing areas. A total of 40 volatile components were identified, and the relative content of volatile components in Artemisiae Argyi Folium was significantly different among the samples from different Dao-di producing areas. The principal component analysis and partial least squares discriminant analysis identified 8 volatile components as the potential markers for discrimination of Artemisiae Argyi Folium samples from different Dao-di producing areas. This study revealed the differences in the chemical composition of Artemisiae Argyi Folium samples from three different Dao-di producing areas, providing analytical methods and a scientific basis for the discrimination and quality evaluation of Artemisia Argyi Folium in different Dao-di producing areas.
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Gas Chromatography-Mass Spectrometry , Chromatography, High Pressure Liquid/methods , Drugs, Chinese Herbal/chemistry , Flavonoids/analysis , Plant Leaves/chemistry , Artemisia/chemistryABSTRACT
ObjectiveTo compare the effects of different drying methods on volatile components of Pseudostellariae Radix. MethodThe samples were dried by different methods, including air drying, sun drying, hot air drying (40, 60, 80 ℃) and vacuum freeze drying. Gas chromatography-ion mobility spectrometry (GC-IMS) was used to compare the changes of volatile components in the samples after different treatments. The samples were incubated at 80 ℃ and 500 r·min-1 for 15 min, the injection temperature was 85 ℃, the injection volume was 200 μL, the flow rate of carrier gas was from 2 mL to 150 mL during 20 min, and the temperature of IMS detector was 60 ℃. SE-54 capillary column (0.32 mm×30 m, 0.25 μm) was used, the column temperature was 60 ℃, and the analysis time was 35 min. The differential spectra of volatile components were constructed and analyzed by principal component analysis (PCA). ResultA total of 37 volatile components were identified from dried Pseudostellariae Radix. The number of compounds in descending order was ketones, aldehydes and alcohols. There were some differences in the volatile components in samples dried by different methods. And the volatile components in samples with sun drying, air drying and hot air drying at 40 ℃ were similar, compared with other drying methods, vacuum freeze drying and hot air drying at 80 ℃ had great effects on the volatile components of Pseudostellariae Radix, and the compounds in the samples with vacuum freeze drying were the least. ConclusionIn this study, GC-IMS for the detection and analysis of volatile components in Pseudostellariae Radix is established, which has the characteristics of high efficiency, nondestructive inspection and simple sample processing. This method can be used for the distinction of Pseudostellariae Radix dried by different methods. And hot air drying at 40 ℃ can effectively retain the volatile components of Pseudostellariae Radix, and achieve similar flavor to samples with sun drying and air drying.
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ObjectiveTo analyze the quality changes of Platycladi Semen before and after the deterioration of moth-eaten and rancidity during storage. MethodFour types samples of Platycladi Semen, including normal, moth-eaten, oxidative rancidity and hydrolytic rancidity, were determined for volatile components, odor, and taste based on headspace solid phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) and electronic sensory techniques such as electronic nose and electronic tongue. Volatile components were identified by searching the database and manual comparison, the odor and taste were determined by the response values of the electronic nose and electronic tongue sensors, and the difference between samples before and after deterioration was studied by multivariate statistical analysis. ResultA total of 85 compounds were identified in Platycladi Semen samples. Compared with the normal samples, the number of volatile compounds in samples after hydrolytic rancidity decreased by 5, the number of volatile compounds in samples after moth-eaten and oxidative rancidity increased by 1 and 21, respectively. Aldehydes and acids accounted for majority of types. Among them, the contents of N-hexanoic acid, hexanal and propionic acid in the samples of oxidative rancidity reached 11.49%, 10.21% and 7.52%, which became the key indicators of rancidity. There was significant variance among the odor components corresponding to W1W, W2W and W1S sensors by electronic nose analysis. It was indicated that the value of sourness in deteriorated samples generally increased by mean of electronic tongue analysis. Compared with normal samples, the moth-eaten samples had changed slightly and rancidity samples had changed significantly especially oxidative rancidity samples of volatile components, odor and taste by multivariate statistical analysis. ConclusionIn terms of Platycladi Semen, the oxidative rancidity caused by nature storage for 12 months has the greatest impact on the quality. Therefore, it should be mainly to prevent oxidative rancidity to ensure the quality of Platycladi Semen.
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OBJECTIVE To optimize the extraction technology of volatile components from Wuyao decoction. METHODS On the basis of single factor investigation ,the extraction technology of volatile components from Wuyao decoction was optimized and validated by Box-Behnken design-response surface technology using the contents of bomyl acetate ,cyperotundone,α-cyperone, ligustilide and dehydrocostuslactone , extraction rate of volatile oil as indexes , with extraction time , soaking time and liquid-material ratio as factors. On this basis ,the extraction state of the decoction was quantified. RESULTS The optimal extraction technology was as followed :the ratio of liquid -material was 13∶1(mL/g),soaking time was 0.5 h,and the extraction time was 6 h in the boiling state. The comprehensive scores of the three validation experiments were 0.948 7,0.948 4 and 0.948 6 respectively (RSD=0.02%,n=3),and the deviation from the predicted value (0.947 9)was no more than 1%. The boiling state of the decoction in 180 ℃ oil bath was taken as the sudden boiling state. CONCLUSIONS The optimized extraction technology is stable and feasible.
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ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water, the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea, and their processed products of rice-washed water. Chromatographic conditions were programmed temperature (starting temperature of 50 ℃ for 2 min, rising to 120 ℃ with the speed of 10 ℃·min-1, then rising to 170 ℃ at 2.5 ℃·min-1, and rising to 240 ℃ at 10 ℃·min-1 for 3 min), the inlet temperature was 280 ℃, the split ratio was 10∶1, and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization (EI) with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discriminant analysis (OPLS-DA) on each sample data, the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection (VIP) value>1. ResultA total of 60 components were identified, among which 40 were rhizomes of A. chinensis and 38 were its processed products, 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively, indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water, and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same, but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids, and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water, the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed, and pinene, 3-carene, p-cymene, ocimene, terpinolene, atractylon, acetic acid and furfural can be used as difference markers before and after processing.
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ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water, the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea, and their processed products of rice-washed water. Chromatographic conditions were programmed temperature (starting temperature of 50 ℃ for 2 min, rising to 120 ℃ with the speed of 10 ℃·min-1, then rising to 170 ℃ at 2.5 ℃·min-1, and rising to 240 ℃ at 10 ℃·min-1 for 3 min), the inlet temperature was 280 ℃, the split ratio was 10∶1, and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization (EI) with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discriminant analysis (OPLS-DA) on each sample data, the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection (VIP) value>1. ResultA total of 60 components were identified, among which 40 were rhizomes of A. chinensis and 38 were its processed products, 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively, indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water, and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same, but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids, and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water, the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed, and pinene, 3-carene, p-cymene, ocimene, terpinolene, atractylon, acetic acid and furfural can be used as difference markers before and after processing.
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ObjectiveTaking Chuanxiong Chatiaosan prescription as the carrier, by comparing the differences of volatile components in Chuanxiong Rhizoma with single decoction pieces and compatible prescription of different decoction pieces, the differences of material basic connotation of different formulations of Chuanxiong Chatiaosan were revealed from the aspects of processing (raw and wine-processed products), compound compatibility and dosage form (powder and decoction). MethodThe volatile oil was extracted from different decoction pieces of Chuanxiong Rhizoma, Chuanxiong Chatiaosan and its decoction with different decoction pieces of Chuanxiong Rhizoma by steam distillation, the main components and their relative contents were identified by gas chromatography-mass spectrometry (GC-MS). ResultA total of 25 volatile components were identified from different processed products of Chuanxiong Rhizoma, including 11 monoterpenoids, 4 phenols, 3 sesquiterpenoids, 3 phthalides, 2 ketones and 2 olefins, the contents of α-pinene, β-pinene, 3-butylphthalide and others increased after the raw products was processed with wine. A total of 85 constituents were identified from Chuanxiong Chatiaosan with different decoction pieces, including 31 monoterpenoids, 23 sesquiterpenoids, 5 alcohols, 5 aldehydes, 4 phenols, 4 phthalides, 3 ethers, 3 ketones, 1 olefin, 1 organic acid, 2 esters and 3 other compounds. A total of 22 components, including 9 sesquiterpenoids, 3 phthalides, 2 phenols, 6 monoterpenoids, 1 aldehyde and 1 alkane, were identified from the decoction of Chuanxiong Chatiaosan with different processed products. ConclusionThere was no significant difference in the composition between raw products and wine-processed products of Chuanxiong Rhizoma either in single decoction pieces or in compatibility prescription, but the relative content changed to some extent, and the wine-processed products was the most obvious. There was a great difference in the composition of volatile components between the Chuanxiong Chatiaosan and its decoction. The volatile components, such as isopulegol, isocalamendiol and safrole, were not found in the decoction. Components in Chuanxiong Rhizoma processed with wine will change with the addition of yellow rice wine, and volatile components can reflect the difference between decoction pieces and prescriptions of the wine-processed products.
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ObjectiveBy comparing the difference of volatile components of the decoction pieces before and after being processed by braising method of Jianchangbang and steaming method included in the 2020 edition of Chinese Pharmacopoeia, the influence of processing methods on the flavor formation of Polygoni Multiflori Radix (PMR) was compared. MethodHeadspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components of 30 batches of PMR samples from 3 origins with 3 processing methods. The GC was performed under programmed temperature (starting temperature of 40 ℃, rising to 150 ℃ at 5 ℃·min-1, and then rising to 195 ℃ at 10 ℃·min-1) with high purity helium as carrier gas and the split ratio of 10∶1. Mass spectrometry conditions were electron impact ion source (EI) and the detection range of m/z 50-650, the peak area normalization method was used to calculate the relative mass fraction of each component. The chromaticity values of different processed products were measured by a precision colorimeter, the relationship between chromaticity values and relative contents of volatile components was investigated by OriginPro 2021, principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed on the sample data by SIMCA14.1. The differential components of different processed products of PMR were screened according to the principle of variable importance in the projection (VIP) value>1.5, and the material basis of different odor formation of PMR and its processed products was explored. ResultA total of 59 volatile components were identified, among which 34 were raw products, 33 were braised products, and 27 were steamed products. PCA and OPLS-DA results showed that there were significant differences between the three, but there was no significant difference between samples from different origins of the same processing method. Color parameters of a*, b*, E*ab had no significant correlation with contents of volatile components, while L* was negatively correlated with contents of 2-methyl-2-butenal, 2-methyltetrahydrofuran-3-one and 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one (P<0.05). The contents of pungent odor components such as caproic acid, nonanoic acid and synthetic camphor decreased after processing, while the contents of sweet flavor components such as 2-methyl-2-butenal, furfural and 5-hydroxymethylfurfural increased after processing, and the contents of furfural, 5-methyl-2-furanmethanol, 5-hydroxymethylfurfural and other aroma components in the braised products were significantly higher than that in the steamed products. ConclusionHS-GC-MS can quickly identify the volatile substance basis that causes the different odors of PMR and its processed products. The effect of processing methods on the odor is greater than that of origin. There is a significant correlation between the color parameter of L* and contents of volatile components, the "raw" taste of PMR may be related to volatile components such as caproic acid, pelargonic acid and synthetic camphor, the "flavor" after processing may be related to the increase of the contents of 2-methyl-2-butenal, furfural, 5-hydroxymethylfurfural, methyl maltol and furfuryl alcohol.
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The volatile oil of Chuanxiong Rhizoma(CX) is known as an effective fraction. In order to seek a suitable method for processing CX and its decoction pieces, this study selected 16 volatile components as indices to investigate how different processing methods such as washing/without washing, sun-drying, baking, oven-drying and far-infrared drying at different temperatures affected the quality of CX and its decoction pieces(fresh CX was partially dried, cut into pieces, and then dried) by headspace gas chromatography-mass spectrometry(GC-MS), cluster analysis, principal component analysis and comprehensive weighted scoring. The results showed that the rapid washing before processing did not deteriorate the volatile components of CX. Considering the practical condition of production area, oven-drying was believed to be more suitable than sun-drying, baking, and far-infrared drying. The CX decoction pieces with a thickness of 0.3-0.4 cm were recommended to be oven-dried at 50 ℃. The integrated processing(partial drying, cutting into pieces, and drying) did not cause a significant loss of volatile components. For the fresh CX, the oven-drying at 60 ℃ is preferred. The temperature should not exceed 60 ℃, and drying below 60 ℃ will prolong the processing time, which will produce an unfavorable effect on volatile components. This study has provided the scientific evidence for field processing of CX, which is conducive to realizing the normalization and standardization of CX processing in the production area and stabilizing the quality of CX and its decoction pieces.
Subject(s)
Desiccation , Gas Chromatography-Mass Spectrometry/methods , Oils, Volatile , Principal Component Analysis , Rhizome/chemistry , Volatile Organic Compounds/analysisABSTRACT
Objective:The volatile components of Rhododendri Mollis Flos were determined and the differences of volatile components at different flowering stages were compared and analyzed. Method:Gas chromatography-ion mobility spectrometry (GC-IMS) was used to detect the volatile components in Rhododendri Mollis Flos at different flowering stages (bud stage, initial flowering stage, half-flowering stage, blooming stage and late blooming stage). GC-IMS spectra combined with cluster analysis, principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used to compare the differences and similarities of volatile components in different flowering stages. Result:A total of 70 volatile components in Rhododendri Mollis Flos at different flowering stages were detected, among which 67 were common components, and 47 were identified qualitatively, mainly alcohols, esters and aldehydes. Carveol was a special component at the late blooming stage. The content of alpha-terpineol is the highest at the initial flowering stage, but not at the blooming stage and late blooming stage. The relative contents of the active ingredients [6-methyl-5-hepten-2-one, nonanal, alpha-terpineol, 1,8-cineole, linalool oxide, 1-octen-3-ol, (<italic>E</italic>)-3-hexenol] showed a decreasing trend during flowering stages. GC-IMS spectra showed that the samples at different flowering stages had their own characteristic peak regions, and also had common regions. The results of cluster analysis, PCA and OPLS-DA all showed that the samples at different flowering stages were distinguishable. OPLS-DA was used to screen 19 different components to distinguish different flowering stages, including <italic>γ</italic>-butyrolactone, 1,8-cineole, ethyl hexanoate, etc. Conclusion:Rhododendri Mollis Flos samples at different flowering stages can be distinguished obviously, and the active substances in the volatile components are gradually dissipated with the degree of flower opening, which can provide reference for the improvement of material basis and the study of different flowering stages of Rhododendri Mollis Flos.
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Asari Radix et Rhizoma (ARR) is a traditional Chinese medicine for relieving exterior syndrome, and its roots and stems contain rich chemical components, including volatile oils (terpenoids, aromatics and aliphatics), lignans, flavonoids, etc. Clinically, it has been traditionally used for the treatment of diseases such as phlegm and cough, anemofrigid cold, rheumatic arthralgia due to its ability to spread cold. Modern pharmacological studies have shown that ARR played beneficial roles in analgesic, anti-inflammatory, antitussive, antiasthmatic, antiviral, antibacterial, sedative, antioxidative, and antidepressant responses, antihypertension, as well as tumor suppression. The current studies on the chemical composition of ARR mainly focused on volatile components, and little information is available for the occurrence and pharmacological effects of non-volatile components. In addition, there is a lack of clear classification of chemical components and the distribution of chemical components in medicinal parts and the origin of species. Therefore, in this study, the authors reviewed a large number of literature on the chemical compositions and pharmacological effects of ARR, and hoping to provide a reference for further pharmacological research and the new drug development of ARR.
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Objective:To compare the effects of different drying methods on the chemical constituents of Trichosanthis Fructus. Method:Trichosanthis Fructus was dried by means of air drying, sun drying, hot air drying (40, 60, 80 ℃) and variable temperature drying (50-80, 80-50 ℃). The contents of nucleosides and flavonoids in Trichosanthis Fructus peels and seeds treated by different methods were compared by high performance liquid chromatography (HPLC), mobile phase was acetonitrile-0.2% acetic acid aqueous solution (3∶7) (A)-acetonitrile (B) for gradient elution (0-15 min, 97-95%B; 15-30 min, 95%-90%B; 30-35 min, 90%-87%B; 35-40 min, 87%-86.5%B; 40-48 min, 86.5%-97%B; 48-50 min, 97%B), the detection wavelength was 260 nm, and the flow rate was 0.4 mL·min<sup>-1</sup>. Gas chromatography-ion mobility spectrometry (GC-IMS) was used to compare the changes of volatile components in the samples treated by different treatments. The volatile components were incubated on a SE-54 capillary column (0.32 mm×30 m, 0.25 μm) at 80 ℃ and 500 r·min<sup>-1</sup> for 15 min, the injection temperature was 85 ℃, the injection volume was 400 μL, the analysis time was 35 min, carrier gas was high purity nitrogen, the flow rate of carrier gas was 2.0 mL·min<sup>-1</sup>, the flow rate of drift gas was 150 mL·min<sup>-1</sup>, and the temperature of IMS detector was 45 ℃. Result:The contents of uridine, adenosine and adenine were higher after hot air drying at >50 ℃. Low temperature drying was conducive to maintaining the stability of cytidine, cytosine, rutin, luteolin and 2ʹ-deoxyadenosine. GC-IMS technology could realize the analysis and identification of Trichosanthis Fructus samples after different treatments. There were more volatile components after hot air drying at 80 ℃ and variable temperature drying. Conclusion:Hot air drying at 40 ℃ and 60 ℃ can retain nucleosides and flavonoids, and the volatile components are similar to those in traditional drying methods, which has the advantages of high efficient, controllable and suitable for industrial production.
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Objective:To establish and apply a new practical analytical method for identifying the fishy odor of Cordyceps based on headspace-solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry (HS-SPME/GC-QQQ-MS/MS) technique. Method:The InertCap Pure-WAX capillary column (0.25 mm×30 m, 0.25 μm) was used for chromatographic separation. The injection port temperature was set at 250 ℃. The injection mode was split injection with a ratio of 5∶1. High purity helium was used as the carrier gas and control mode was set to constant pressure. The column flow rate was 1.43 mL∙min<sup>-1</sup>, the linear velocity was 43.3 cm∙s<sup>-1</sup>, and the purge flow rate was 3.0 mL∙min<sup>-1</sup>. The chromatographic column temperature program as follows:maintained the initial temperature at 50 ℃ for 5 min, and increased the temperature at a rate of 10 ℃∙min<sup>-1</sup> to 250 ℃, held for 10 min. The column equilibrium time was 2.0 min. The ion source of mass spectrographic analysis was electron ionization with ion source temperature of 200 ℃, and the monitoring mode was set to multiple reaction monitoring. Result:Seven batches of Cordyceps samples were collected, including 3 batches from Sichuan, 3 batches from Qinghai and 1 batch from Tibet. There were six batches of counterfeits, including 3 batches from Sichuan, 2 batches from Guizhou and 1 batch in Xinjiang. A total of 81 volatile compounds were screened out in Cordyceps, which could be divided into 13 types (esters, ketones, aldehydes and others) according to the compound structure, indicating that the fishy odor of Cordyceps was a complex odor. There was no significant difference in the types of volatile compounds of Cordyceps from different regions, which suggested that these volatile compounds in Cordyceps produced in Tibet (Naqu), Qinghai (Yushu and Guoluo) and Sichuan (Litang, Rangtang and Seda) were relatively consistent. However, the contents of some volatile compounds in Cordyceps produced in different regions were quite different, and 16 volatile compounds with significant difference were screened out, including 1-methoxy-2-propyl acetate, <italic>γ</italic>-octalactone, hexyl acetate and others, those compounds maybe could been used as the quality markers for identification of regions of Cordyceps. There was a large difference in volatile compounds between Cordyceps and its counterfeits, and 34 volatile compounds were screened out, including ethyl acetate, acetophenone, 2-ethyl-1-hexanol and others, those compounds maybe could been used as the quality markers for authenticity identification of Cordyceps. Conclusion:In summary, the established method for identifying the fishy odor of Cordyceps in this paper has the characteristics of high sensitivity, accuracy and simplicity, which can provide reference for the analysis of volatile compounds in other Chinese herbal medicines.
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Considering the characteristic chromatograms and quality value transmitting of three volatile components, this study investigated the changes in volatile components of Menthae Haplocalycis Herba in each heating process of personalized preparations and identified the critical control points for the application of volatile components from traditional Chinese medicine in such preparations. The characteristic chromatograms of volatile components in Menthae Haplocalycis Herba were established by gas chromatography, followed by the quantitative determination of three volatile components menthone, menthol, and piperitone and the comparison of retention rates of volatile components during the crushing, extraction, concentration and drying of preparation products and their change rules in characteristic peaks. The results showed that the volatile components of Menthae Haplocalycis Herba were reduced in each process. The loss rate was low in the crushing process when the volatile component peaks were present, but high in the extraction and concentration processes, manifested as the absence of partial component peaks and the presence of new component peaks. The changes in volatile components of Chuanxiong Chatiao Granule in the drying process were compared with those in Chuanxiong Chatiao Pill, both of which were prepared from the raw Menthae Haplocalycis Herba powder, and the findings demonstrated that Chuanxiong Chatiao Pill was superior to Chuanxiong Chatiao Granule. This study confirmed that the retention rates of volatile components in Menthae Haplocalycis Herba were mostly affected by the extraction and concentration processes, and the packing of preparations helped to reduce the loss of volatile components in Menthae Haplocalycis Herba powder, which has provided reference for the application of Chinese medicinal materials containing volatile components in the personalized preparations.
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Drugs, Chinese Herbal , Medicine, Chinese Traditional , PowdersABSTRACT
OBJECTIVE:To analyze the chemotypes of volatile components from Perillae Folium of different germplasms ,and to investigate the relationship of germplasm and leaf color with chemotype. METHODS :The fingerprints of volatile components from 30 batches of Perillae Folium were prepared by GC-MS with P 4 peak as reference. Similarity Evaluation System for TCM Chromatographic Fingerprint (2004A edition )was applied to evaluate the similarity and confirm common peaks. The volatile components of Perillae Folium were determined by the same GC-MS method. Qualitative Navigator (B.08.00)software was used to analyze and compare with NIST 17.0 standard mass spectrum database. The compounds corresponding to the peak were analyzed ; clustering analysis was carried out with Origin 2018 software. RESULTS :There were 13 common peaks in the fingerprints of volatile components from 30 batches of Perillae Folium . The similarities were 0.13-1.00. Totally 54 components were identified from 30 batches of Perillae Folium of different germplasm. Cluster analysis showed that 30 batches of Perillae Folium samples could be clustered into three categories ;among them ,SCY-1,YNT-9,YNX-17,YN-28 were clustered into one category ,with phenylpropanoid-elemicin(PP-e as )the main volatile component ,being PP-e type ;GS-4,GS-7,GS-11,GS-19,HBA-14, HBA-20,GZZ-8,LN-39,GSL-27,GSQ-32,GSQ-33,GST-31,YNW-12,LN-38 were clustered into one category ,and the content of perilla ketone (PK)in them was the highest except for LN- 38, being PK type [the content of phenylpropanoid-apiol(PP-a)in LN- 38 was higher than that of perilla ketone ,being PP-a type] ;HBS-2,HBS-3,HBS-6, C201859)HBS-15,HBS-16,HBS-24,HBS-25,GX-26,SXS-30,SCC- 36,RB-37,SC-29 were clustered into one category ,and thecontent of perillaldehyde (PA)was the highest ,being PA type.The color characteristics of Perillae Folium of different germplasm showed that Perilla frutescens (L.) Britt. var.frutescens with green leaves on both sides was PK type ,while P. frutescens (L.)Britt. var. arguta with purple leaves on one or both sides was PA type ,and P. frutescens (L.) Britt var. auriculato-dentata C. Y. Wu et Hsuan ex H. W. Li was PP-e type. CONCLUSIONS:The chemotype of volatile components in Perillae Folium have a certain corresponding relationship with their leaf colors. Most of P. frutescens (L.)Britt. var. arguta with purple leaves on one side or both sides are PA type. P. frutescens (L.) Britt. var. acuta (Thunb.)Kudo,P. frutescens (L.)Britt var. auriculato-dentata C. Y. Wu et Hsuan ex H. W. Li and P. frutescens (L.)Britt. var. frutescens with green leaves on both sides do not belong to PA type ,among which P. frutescens (L.)Britt var. frutescens is PK type ,while P. frutescens (L.)Britt var. auriculato-dentata C. Y. Wu et Hsuan ex H. W. Li is mostly PP-e type.