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Objective: To compare the differences of Gardeniae Fructus and its stir-baked preparation and screen out the differential markers, and provide reference for the establishment of quality standard. Methods: The whole and partial fingerprints of Gardeniae Fructus and its stir-baked prepared slices were established by HPLC-UV analysis. And the fingerprints were statistically analyzed using hierarchical clustering analysis (HCA), principle component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA), then the characteristic markers were screened out. And then content of 6-α-hydroxygeniposide, gentioside, geniposide, crocin I, and crocin II was determined. Results: A total of 15 peaks were acquired for Gardeniae Fructus and stir-baked Gardeniae Fructus respectively, 12 peaks of which were the common peaks. The similarity of whole and partial reference fingerprints of Gardeniae Fructus and its stir-baked prepared slices was 0.991 and 0.880, respectively, and partial fingerprint can successfully distinguished Gardeniae Fructus from its stir-baked prepared slices. HCA and OPLS-DA results showed that significant differences were observed between Gardeniae Fructus and stir-baked Gardeniae Fructus with peak 3, peak 5, peak 9 (geniposide), and peak 11 (crocin I), which being identified as the main differential markers. Contents of geniposide, crocin I and crocin II in Gardeniae Fructus were higher than those in stir-baked Gardeniae Fructus, while 6-α-hydroxygeniposide was lower. Conclusion: The composition was significantly different before and after stir-baked. The established partial fingerprints combined with multi-component determination method can effectively distinguish them. And the differential markers obtained by multivariate statistical analysis can provide reference for the selection of quality markers.
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Objective: To evaluate the quality of Gardeniae Fructus from different producing areas and optimize the best place of production by using chemical pattern recognition method based on HPLC fingerprint and multi-component content determination. Methods: The RP-HPLC using acetonitrile-0.1% phosphoric acid aqueous solution as mobile phase based on the wavelength switching (234 nm and 440 nm) and gradient elution method was developed to evaluate the quality of 30 batches of Gardeniae Fructus from 10 different producing areas. The combination of chromatographic fingerprints and quality determination of five active ingredients, as well as chemometrics including hierarchical cluster analysis (HCA) and principal component analysis (PCA), were further employed for the quality assessment. Results: The fingerprint similarity of 30 batches of Gardeniae Fructus from 10 different producing areas were all above 0.95. The content ranges of deacetylated methyl oxalate, genipin gentiobioside, geniposide, crocin I, and crocin II were 0.61-4.26 mg/g, 1.73-12.92 mg/g, 51.79-82.76 mg/g, 5.03-12.80 mg/g, and 0.71-2.28 mg/g. Samples can be divided into three categories by HCA: The first category is Yongzhou in Hunan, Yong’ an in Hunan, Fengcheng in Jiangxi, Hukou in Jiangxi, Guangde in Anhui, and Fuding in Fujian; The second category is Lichuan in Jiangxi, Jurong in Jiangsu and Tanghe in Henan; And the third category is Lu’ an in Anhui. PCA was used to further evaluate the quality differences of the samples from different producing areas, and it was found that the medicinal materials from Lu’ an in Anhui, Hukou in Jiangxi, and Yong’ an in Hunan were of superior quality. Conclusion: The quality of Gardeniae Fructus from different producing areas was different to a certain extent, while the quality of same batches was stable. By combination of fingerprint and content determination, the chemical pattern recognition method can be used to evaluate the quality of the Gardeniae Fructus comprehensively. The establishment of this method provided an effective reference for the quality control and evaluation of Gardeniae Fructus.
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Objective To find the constituents that is closely related to the color change during the stir-frying process of Gardeniae Fructus Praeparatus (Jiaozhizi in Chinese herbal name, JZZ). Methods The colorimetric method was used to measure the chromatic value of the samples during the stir-frying process of JZZ. High performance liquid chromatography (HPLC) was used to determine the common constituents of samples in the processing of JZZ, and the multivariate statistical methods of correlation and discriminant analysis was used to investigate the color and constituents of JZZ. Results The E* ab of eight constituents in processed JZZ samples showed a highly linear positive correlation, they were gardoside, crocin-I, crocin-II, p-coumaroylgenipin gentiobioside, I6, I12, C1 and C2. The contents of these eight components decreased with the increase of color in the stir-frying process. Ten key components of JZZ samples, scandoside methyl ester, deacetyl asperulosidic acid methyl ester, gardoside, crocin II, crocin I, peaks C1, C2, C4, C6, and C7,had significant changes in contents. Conclusion Gardoside, crocin I and crocin II are the most important components in the stir-frying process of JZZ, which are highly correlated with the change of color and can be used as chemical markers for the quality control of JZZ.
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Objective To establish the multi-wavelength fusion HPLC fingerprints of Gardeniae Fructus and to make quantitative analysis of the common peaks by ESI-Q-TOF MS. Methods The Kromasil 100-5 C18 column was used with a mobile phase of acetonitrile-0.1% phosphoric acid in gradient elution; The flow rate was 1.0 mL/min; The column temperature was 35 ℃; The detection wavelength was 238, 327, and 440 nm. Matlab7.1 was adopted for multi-wavelength fusion of the data in CSV format. Results Twenty chemical constituents were detected in fusion fingerprint, which included more information. Sixteen chemical constituents were compared with reference standards and identified by MS. The similarity of 10 batches of Gardeniae Fructus was over 0.90. Conclusion The systematic quantified fingerprint method based on the technique of multi-wavelength fusion fingerprint and identifying 16 constituents can be used for the fully quality control of Gardeniae Fructus.
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OBJECTIVE: To study the chemical constituents from the flower buds and inflorescences of Buddleja officinalis. METHODS: Various chromatographic techniques such as silica gel and Sephadex LH-20 chromatography were used in this experiment. RESULTS: Sixteen compounds were isolated from the medicinal plant, and their structures were identified as follows acacetin(1), apigenin(2), luteolin(3), acacetin-7-O-glucoside(4), cosmosiin(5), luteolin-7-O-glucoside(6), acacetin-7-O-glucuronide(7), apigenin-7-O-glucuronide(8), linarin(9), luteolin-7-O-rutinoside(10), neobudofficide(11), acteoside(12), crocin III(13), crocin II(14), crocin I(15), and N1, N5, N10-(E)-tri-p-coumaroylspermidine(16). CONCLUSION: Compounds 4, 7, 8, 14-16 are obtained from the medicinal plant for the first time, and compounds 7, 8, 14-16 are obtained from Loganiaceae for the first time.
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Objective: To establish an HPLC-DAD method for the simultaneous determination of eight components in Jiaowei Xiaoyao Pill (JXP), such as jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid. Methods: The chromatographic separation was performed on a Plastisil ODS column (250 mm×4.6 mm, 5 μm) with acetonitrile (B)-0.2% phosphate acid solution (D) as mobile phase at the flow rate of 1.0 mL/min for gradient elution and the column temperature was 37℃. The detection wavelength was set at 238 nm for jasminoidin, 274 nm for liquiritin and paeonol, 440 nm for crocin I and crocin II, 228 nm for peoniflorin and glycyrrhizic acid, and 324 nm for ferulic acid. The volume of sample injection was 10 μL. Results: The eight compounds were well separated under the determined chromatographic conditions. The RSD of precision and repeatability experiment were all less than 2% and the sample solution was stable during 12 h. All the compounds had a wide linear range and good linearity: the linear range of jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid were 48-288 μg/mL (r=0.9994), 60-360 μg/mL (r=0.9992), 64-384 μg/mL (r=0.9998), 19.2-115.2 μg/mL (r=0.9995), 4-24 μg/mL (r=0.9992), 96-576 μg/mL (r=0.9996), 64-384 μg/mL (r=0.9997), and 20-120 μg/mL (r=0.9994), respectively. The average recoveries were between 99.13%-100.25% and the RSD were all less than 2.0%. The content ranges of jasminoidin, liquiritin, paeonol, crocin I, crocin II, peoniflorin, glycyrrhizic acid, and ferulic acid in six batches of JXP were 2.34-2.82 mg/g, 2.63-3.28 mg/g, 3.66-4.55 mg/g, 1.05-1.41 mg/g, 0.34-0.41 mg/g, 4.78-5.32 mg/g, 2.83-3.37 mg/g, and 1.36-1.73 mg/g, respectively. Conclusion: The method is simple and convenient, and the methodology validation shows that determination result of the method is accurate and reliable and it can be an effective approach for the quality control of JXP.
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Objective: To develop an UPLC-DAD method for simultaneous determination of gallic acid, cinnamic acid, licorice glycosides, crocin I, crocin II, cinnamic aldehyde, eugenol, glycyrrhetinic acid, and muscone in Zhenlong Xingnao Capsule. Methods: Analysis was performed on a RP-UPLC method and an Agilent Zorbax C18 chromatographic column (100 mm × 2.1 mm, 1.8 μm) eluted with 0.1% formic acid (mobile phase A) and acetonitrile (mobile phase B), the flow rate was 0.3 mL/min, gradient elution and column temperature was 35℃, the injection volume was 1 uL. Respectively to measure their extraction solvent, linear range, precision, repeatability, stability, and recovery rate. Results: The nine components were well separated and showed good linearity, such as gallic acid 0.2-20.0 mg/L (r = 0.999 0), crocin I 0.022-2.200 mg/L (r = 0.999 3), crocin II 0.02-2.00 mg/L (r = 0.999 6), licorice glycosides 0.093-1.860 mg/L (r = 0.999 4), cinnamic acid 0.020 4-2.040 0 mg/L (r = 0.999 9), cinnamic aldehyde 0.042-4.200 mg/L (r = 0.999 9), eugenol 0.95-95.00 mg/L (r = 0.999 9), glycyrrhetinic acid 0.012 9-1.290 0 mg/L (r = 0.998 9), and muscone 0.073 8-7.380 0 mg/L (r = 0.999 0). The precision was good, RSD was 1.02% or less, The repeatability is good in terms of RSD of 1.13% or less and the recovery rate was 93.8%-112.1% (RSD 1.28% or less). Test solution was stable at room temperature within 24 h. The contents of three batches of the gallic acid, crocin I, crocin II, licorice glycosides, cinnamic acid, cinnamic aldehyde, eugenol, glycyrrhetinic acid, and muscone were 0.422-0.448, 0.093-0.105, 0.096-0.112, 0.026 8-0.028 5, 0.142-0.153, 0.140-0.158, 1.519-1.547, 0.007 55-0.008 04, 0.117-0.121 mg/g, respectively. Conclusion: The method is rapid and has high sensitivity, high accuracy, and good specificity, It can be applied to the quality control of Zhenlong Xingnao Capsule.
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Objective: To compare the changes of seven kinds of compounds in the fruits, seeds, and peels of Gardeniae Fructus. Methods: Quantitative analysis of geniposidic acid, deacetyl asperulosidic acid methyl ester, genipin-1-gentiobioside, geniposide, chlorogenic acid, crocin I, and crocin II in the fruits, seeds, and peels of Gardeniae Fructus with rocessed and no processed, were firstly carried out by HPLC/DAD. Results: The conents of deacetyl asperulosidic acid methyl ester and chlorogenic acid were higher in the peels of Gardeniae Fructus. The conents of genipin-1-gentiobioside, geniposide, crocin I, and crocin II were higher in the seeds of Gardeniae Fructus. Geniposidic acid content was increased in turn, the content of deacetyl asperulosidic acid methyl ester, geniposide, chlorogenic acid, crocin I, and crocin II were reduced in turn and genipin-1-gentiobioside contents were not changed from crude, stir-fired, and stir-baked products. Conclusion: The contents of eacetyl asperulosidic acid methyl ester, genipin-1-gentiobioside, geniposide, chlorogenic acid, crocin I, and crocin II between the seeds and peels of Gardeniae Fructus exist differences. The main ingredients of Gardeniae Fructus are decreased after processing except the increasing of geniposidic acid.