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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 establish HPLC fingerprints for the identification of Ilicis Rotundae Cortex (Jiubiying), dried bark of Ilex rotunda Thunb., and its adulterant, dried bark of Ilex godajam (Colebr.) Wall.. Methods Some samples named Jiubiying were collected from some medicine markets and drugstores. The HPLC fingerprints were obtained to detect Jiubiying and Ilex godajam. The software Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine (2004A edition) was used to evaluate fingerprints. Results The fingerprints of Jiubiying and Ilex godajam were established. Methodological study met the technical requirements of fingerprints. There were 31 and 28 common peaks in Jiubiying and Ilex godajam, respectively. Jiubiying and Ilex godajam could be classified into two clusters by principal component analysis and hierarchical clustering analysis. Conclusion Jiubiying and Ilex godajam can be identified by HPLC fingerprints. This method can provide an effective method for quality evaluation of Jiubiying.
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Objective To evaluate the quality coherence of commercial Angelicae Dahuricae Radix (Baizhi) decoction pieces. Methods The samples of 12 batches of commercial decoction pieces, 1 batch of sulphur fumigated Baizhi, and 1 batch of naturally dried Baizhi were collected. HPLC method was used to determine the fingerprints and the contents of imperatorin and isoimperatorin by C18 column (4.6 mm×250 mm, 5 μm) with a gradient mobile phase of acetonitrile-water solution system at the flow rate of 1.0 mL/min. The column temperature was set at 35 ℃, and the max plot of detection wavelength was in 210-800 nm. Similarity calculation was used to analyze the data. Results The HPLC fingerprint analysis method was established with 12 common peaks. The similarities of 12 batches of commercial decoction pieces of Baizhi were 0.840-0.973. Their similarities compared with the sulphur fumigated Baizhi were 0.672-0.908. Compared with naturally dried Baizhi, the similarities of fingerprint were 0.536-0.684. The contents of imperatorin and isoimperatorin in 12 batches of commercial decoction pieces were 0.035%-0.140% and 0.028%-0.069%, respectively. Conclusion The quality of Baizhi decoction pieces was consistent. It can be speculated that Baizhi decoction pieces were processed with sulphur fumigation.
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Objective To study the correlation between storage time and the content of 5-hydroxymethylfurfural (5-HMF) in Corni Fructus because of the color change caused by storage time. Methods Corni Fructus samples of different storage time with 0, 1, 2, 3, and 4 years were collected. The contents of 5-HMF were determined by HPLC. Results The HPLC determination method of 5-HMF in Corni Fructus was established. The contents of 5-HMF varied from undetected value to 0.292 8%, with the increase of storage time of 0, 1, 2, 3, and 4 years and the color gradually deepened from red, dark red, reddish brown to brown. The contents of 5-HMF in black wine-prepared Corni Fructus were 0.954 4%-1.837%. Conclusion The browning of Corni Fructus is related to the production of 5-HMF. With the extension of storage time of Corni Fructus, the color gradually deepens and the content of 5-HMF increase significantly. The storage time of Corni Fructus can be suggested to be one year.
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Objective To study whether sulphur fumigation can cause changes to the content of imperatorin in Angelicae Dahuricae Radix (Baizhi).Methods The fresh samples of Angelicae Dahuricae Radix were collected from some cultivation bases. Half of each batch root was fumigated with sulfur according to the conventional method, and another half was cut into slices and dried naturally (i.e. without sulfur fumigation). The content of imperatorin was determined by HPLC on C18 column (4.6 mm×250 mm, 5μm) with a gradient mobile phase of acetonitrile-water solution system at the follow rate of 1.0 mL/min, 35℃ of the column temperature, and the max plot in 210-800 nm of the detective wavelength.ResultsTotally 29 batches of fresh roots ofAngelica dahurica were collected. The average contents of imperatorin were 0.202% in the Angelicae Dahuricae Radix with sulfur fumigation and 0.120% in the Angelicae Dahuricae Radix without sulfur fumigation. Compared with the corresponding samples without sulfur fumigation, the content of imperatorin in every Angelicae Dahuricae Radix with sulfur fumigation decreased by 6.77%-77.56% with an average decrease of 39.86%.Conclusion The content of imperatorin decreased significantly in every batch of Angelicae Dahuricae Radix with sulphur fumigation. It shows that the sulphur fumigation method was not suitable for producing and processing Angelicae Dahuricae Radix from fresh roots ofA. dahurica.
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Objective To investigate an optimum extracting technology for total glycosides from dried barks of Ilex rotunda Thunb. Methods The yields of pedunculoside and syringin by high performance liquid chromatography (HPLC) determination were taken as the indexes. Some parameters of the extraction technology were evaluated with an L9(3)4 orthogonal design. The optimum extraction parameters were used to extract total glycosides in laboratory. The feasibility was checked by determining the chemical constituents by means of HPLC method. Results The optimum extracting conditions were 12 times volumes of 50% ethanol as the solvent and refluxing 90 min each time for 3 times. An extract yield of total glycosides was 19.5% from barks of Ilex rotunda. Pedunculoside (292 mg/g), syringin (59.5 mg/g), sinapaldehyde glucoside, syringaresinol 4'-O-β-D-glucopyranoside, and syringaresinol 4',4'-di-O-β-D-glucopyranoside were detected in the extract. Conclusion Some glycosides were found in the extract with the optimum extraction technology in laboratory. The extraction technology is practicable and valid.
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<p><b>OBJECTIVE</b>To separate and identify chemical constituents from stem barks of male plants of Populus tomentosa.</p><p><b>METHOD</b>Fresh stem barks of P. tomentosa were extracted with methanol to obtain extracts which were suspended in water and blended successively with petroleum ether, ethyl acetate and n-butanol. Various chromatographic techniques were used to separate and purify the constituents extracted with ethyl acetate and n-butanol fractions. Their structures were identified on the basis of their physicochemical properties and spectral data.</p><p><b>RESULT</b>Twelve compounds were separated with ethyl acetate and n-butanol fractions and identified as benzoic acid (1), daucosterol (2), tremuloidin (3), rhamnocitrin (4), sakuranetin (5), 7-O-methylaromadendrin (6), isograndidentatin A (7), siebolside B (8), sakuranin (9), micranthoside (10), alpha-D-glucopyranose (11), and sucrose (12).</p><p><b>CONCLUSION</b>Compounds 4-12 were separated from this plant for the first time. Of them, compound 10 was separated from this plant genus for the first time.</p>
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Flavonoids , Glucosides , Phenols , Populus , ChemistryABSTRACT
<p><b>OBJECTIVE</b>To compare and analyze volatile constituents from flowers of Trichosanthes kirilowii, in order to point out characteristic differences between female and male flowers.</p><p><b>METHOD</b>Blooming female and male flowers were collected in the same place. Volatile constituents were extracted from the flower by solid phase micro-extraction (SPME), then separated and analyzed by gas chromatography-mass-spectrometry (GC-MS).</p><p><b>RESULT</b>Fifty-two and forty-five chromatographic peaks were separated from the female and male flowers, respectively. Forty seven constituents were identified and their relative percentage compositions were determined with the peak area normalization method. Linalool, alpha-farnesene, benzene methanol, and (Z)-2-methylbutanal oxime were the main volatile constituents. The contents of linalool and alpha-farnesene in female flower were remarkably higher than those in male. In contrast, the content of benzene methanol in male flower was remarkably higher than that in female.</p><p><b>CONCLUSION</b>In the first study on chemical constituents from flowers in genus Trichosanthes, 37 compounds are separated from T. kirilowii. Contents of linalool, alpha-farnesene and benzene methanol show the characteristic differences of volatile constituents contained in male and female flowers of T. kirilowii, which enriches the basic studies on dioecious plant.</p>
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Flowers , Chemistry , Gas Chromatography-Mass Spectrometry , Solid Phase Microextraction , Trichosanthes , Chemistry , Volatile Organic Compounds , ChemistryABSTRACT
<p><b>OBJECTIVE</b>To research the effect of polysorbate 80 (Tween 80) on Yuxingcao injection and volatile oils from Houttuynia cordata.</p><p><b>METHOD</b>1H-NMR spectra of aldehydic and new matter in Yuxingcao injection, volatile oils of H. cordata, and solutions of Tween 80 and volatile oil of H. cordata are determined and compared from various angles of growing origin, storage temperature, and storage time.</p><p><b>RESULT</b>Three aldehydic singlets in 1H-NMR spectra of every volatile oil from 4 aerial part of H. cordata were observed. These aldehydic peaks were basically disappeared and a new peak at delta 8.30 was found in 1H-NMR spectra of the volatile oil solutions in tween 80. Any obvious aldehydic peak in 1H-NMR spectra did not be observed in Yuxincao injection. A weak peak at 8 8.30 was found in 1H-NMR spectra in Yuxincao injection, and the peak high of delta 8.30 was remarked gone up when the injection was stored in 40 degrees C for 1 to 3 months.</p><p><b>CONCLUSION</b>Tween 80 might cause the obvious reduce of aldehydic compounds contents and the production of a novel singal at delta 8.30 in 1H-NMR spectra when it was mixed with the volatile oil from the aerial part of H. cordata. The novel signal at delta 8.30 in 1H-NMR spectra existed in Yuxincao injection and was very small, but was increased remarkably when the Yuxincao injection was stored at 40 degrees C for 1 month at least.</p>
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Chemistry, Pharmaceutical , Drugs, Chinese Herbal , Chemistry , Houttuynia , Chemistry , Oils, Volatile , Chemistry , Plant Oils , Chemistry , Polysorbates , TemperatureABSTRACT
<p><b>OBJECTIVE</b>To study the relation between the content of 5-hydroxymethyl-furfural (5-HMF) and the degree of floating sugar in root of Achyranthes bidentata.</p><p><b>METHOD</b>An HPLC method was applied with a Waters Symmetry C18 3.9 mm x 150 mm (5 microm) column by using methanol-water (12:88) as the mobile phase at a flow rate of 1.0 mL x min(-1) and a UV detection of 280 nm.</p><p><b>RESULT</b>Along with the degree's deepening of floating sugar, the content of 5-HMF varied with the different shades of the sample. The content was 10 times higher in the black sample (highest degree of flowing suger) than that in the yellowish sample (normal). The concentrations of 5-HMT in five yellowish samples of roots of A. bidentata were 0.162 mg x g(-1) to 0.332 mg x g(-1).</p><p><b>CONCLUSION</b>The content increasing of 5-HMF in the root of A. bidentata was related to the degree of flowing sugar.</p>
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Achyranthes , Chemistry , Carbohydrates , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Furaldehyde , Plant Roots , ChemistryABSTRACT
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.
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Objective To establish a method for determination of rutin in Xueguankang Tea. Methods RP-HPLC method and C18 column were used for determination. Methanol-water-acetic acid (40∶60∶1) was the mobile phase with a flow rate of 1.0 mL/min. The detection wavelength was set at 257 nm. Results There was a good linear relationship of rutin within the range of 0.06～0.3 ?g with r=0.999 2. The average recovery of rutin was 98.48 % with RSD=0.87% (n=5). Conclusion This method is convenient,sensitive,accurate and reproducible,and can be used for the quality control of Xueguankang Tea.