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Objective: To explore the potential insecticidal, ovipositor deterrent and antifeedant effects of ethyl acetate extract of the seeds of Senna tora (Syn. Cassia tora) against cowpea weevil (Callosobruchus maculatus). Methods: The activities were evaluated using standard protocols. In these bioassays, the cowpea seeds were used directly as an insect feed. The activity of the extract and isolated compounds were tested at concentrations of 100, 200 and 300 μg/mL and compared to neem oil and cinnamaldehyde (as standard positive controls). Phytochemical analysis of the ethyl acetate extract was done through a number of chromatographic techniques and the structures of the isolated compounds were established through comprehensive spectroscopic analysis including 2D-NMR and ESI-MS studies. Results: Fractionation of the active ethyl acetate extract resulted in the isolation of one known anthraquinone, aurantio-obtusin (1) and a novel compound that was named as cassiatorin (2). Compounds 1 and 2 showed comparable insect antifeedant properties with the positive controls while their insecticidal and ovipositor deterrent effects were far superior to the standard controls. Conclusions: It is thus concluded that Senna tora extracts and the isolated compounds (1 and 2) may be employed in the postharvest management of stored cowpea seeds and as other crop protectants.
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Objective:To explore the potential insecticidal,ovipositor deterrent and antifeedant effects of ethyl acetate extract of the seeds of Senna tora (Syn.Cassia tora) against cowpea weevil (Callosobruchus maculaws).Methods:The activities were evaluated using standard protocols.In these bioassays,the cowpea seeds were used directly as an insect feed.The activity of the extract and isolated compounds were tested at concentrations of 100,200 and 300 μg/mL and compared to neem oil and cinnamaldehyde (as standard positive controls).Phytochemical analysis of the ethyl acetate extract was done through a number of chromatographic techniques and the structures of the isolated compounds were established through comprehensive spectroscopic analysis including 2D-NMR and ESI-MS studies.Results:Fractionation of the active ethyl acetate extract resulted in the isolation of one known anthraquinone,aurantio-obtusin (1) and a novel compound that was named as cassiatorin (2).Compounds 1 and 2 showed comparable insect antifeedant properties with the positive controls while their insecticidal and ovipositor deterrent effects were far superior to the standard controls.Contusions:It is thus concluded that Senna tora extracts and the isolated compounds (1 and 2) may be employed in the postharvest management of stored cowpea seeds and as other crop protectants.
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Objective:To establish the methods for the qualitative identification and content determination of aurantio-obtusin and chrysophanol in Zeju Jiangzhi tablets. Methods:A TLC method was adopted for the qualitative identification, and an HPLC method was used for the content determination. The determination was performed on a Wondasil C18 (250 mm × 4. 6 mm, 5 μm ) column with the mobile phase of acetonitrile -0. 1% phosphonic acid with gradient elution at the flow rate of 1. 0 ml?min-1 , the detection wave-length was 286 nm, the column temperature was 30℃ and the injection volume was 10μl. Results:The TLC spots of aurantio-obtusin and chrysophanol were clear and well-separated without any negative interference. The HPLC experiment results showed the good line-arity within the range of 1. 03-25. 72μg?ml-1(r=0. 999 9) for aurantio-obtusin, and 0. 48-11. 92μg?ml-1(r=0. 999 9) for chry-sophanol. The average recovery was 99. 21% and 98. 85%, and RSD was 0. 70% and 0. 73%, respectively (n=9). Conclusion:The method is simple, accurate and repeatable, which can be used for the qualitative identification and content determination of auran-tio-obtusin and chrysophanol in Zeju Jiangzhi tablets.
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Objective: To establish HPLC-DAD method for the simultaneous determination of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside in Shenqi Shiyiwei Granule (SSG). Methods: The chromatographic separation was achieved on an Waters XBridge-C18 (250 mm × 4.6 mm, 5.0 μm) column with methanol-acetonitrile-water (15:80:5) and methanol-0.1% phosphoric acid (10:90) as mobile phases for gradient elution, at the flow rate of 1.0 mL/min; The column temperature was 35℃. Results: The linear ranges of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.4-8.0 μg/mL (r = 0.999 2), 0.2-4.0 μg/mL (r = 0.999 5), 0.2-4.0 μg/mL (r = 0.999 5), 0.1-2.0 μg/mL (r = 0.999 6), 0.1-2.0 μg/mL (r = 0.999 7), 0.1-2.0 μg/mL (r = 0.999 4), 0.5-10 μg/mL (r = 0.999 2), 0.6-12 μg/mL (r = 0.999 2), 0.4-8.0 μg/mL (r = 0.999 4), 1.0-20 μg/mL (r = 0.999 6), and 0.8-16 μg/mL (r = 0.9993). The average recoveries (n = 6) were 98.1% (RSD = 0.9%), 98.1% (RSD = 1.6%), 99.1% (RSD = 1.6%), 98.3% (RSD = 1.8%), 99.5% (RSD = 1.5%), 99.9% (RSD = 0.6%), 98.5% (RSD = 0.7%), 100.4 (RSD = 0.8%), 101.6% (RSD = 0.4%), 99.7% (RSD = 0.9%), and 101.2% (RSD = 1.1%), respectively. The contents of nine batches of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.081-0.089, 0.261-0.269, 0.060-0.069, 0.038-0.047, 0.030-0.037, 0.042-0.049, 0.420-0.428, 0.141-0.151, 0.178-0.189, 0.107-0.117, and 0.069-0.078 mg/g. The results showed that there was little difference among the batches. Conclusion: The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of SSG.
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Objective: To establish an accelerated solvent extraction(ASE)-HPLC method to determine chrysophanol and aurantio-obtusin in Cassia obtusifolia L.Methods: The optimal extraction conditions were defined by orthogonal tests using ASE.The method was carried out on an ACE Excel C18-PFP column (75 mm×2.1 mm,2.5 μm) with the mobile phase consisting of 0.1% phosphoric acid solution-acetonitrile with gradient elution.The column temperature was 40 ℃,the flow rate was 0.4 ml·min-1, and the detection wavelength was 284 nm. Results: The best process parameters of ASE were as follows:the extraction solvent was methanol, the extraction temperature was 120 ℃ and the static extraction duration was 5 minutes for three cycles.The ASE method needed only 1/9 of the time as the pharmacopoeia method,while the extraction efficiency of the ASE method was higher.The linear ranges of cassia obtusifolia L.and Chrysophanol were at 0.73~58.57 μg·ml-1(r=0.999 7) and 1.09~87.29 μg·ml-1(r=0.999 6).The average recoveries were 102.7%(RSD=0.8%) and 98.2%(RSD=1.5%).Conclusion: The method is simple, rapid and sensitive, which can be used for the rapid determination of aurantio obtusin and chrysophanol in Cassia obtusifolia L.
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Objective:To optimize the extraction parameters for anthraquinones in Semen Cassiae by Box-Behnken experimental design. Methods:Based on single factor screening, a three-factor and three-level Box-Behnken experimental design was employed with the ethanol concentration, material to liquid ratio and extraction time as the independent variables. The dependent variables including the extration rates of chrysophand and aurantio-obtusin were transformed into desirability mathematically by Hassan 's method. The mathematical relationship was established between the dependent variables and the independent variables. The optimum experimental conditions were selected from the stationary point of the response surfaces. Results:The optimum extraction conditions were as follows:12-fold amount of 44％ ethanol as the solvent, extracted three times with 2. 65h for each time. The extraction rate of chrysophanol and aurantio-obtusin was 1. 921％ and 3. 244％, respectively. Conclusion:The measured value is close to the predicted one,which indi-cates the comprehensive extraction parameters optimized by Box-Behnken experimental design can be used for the extraction of chry-sophanol and aurantio-obtusin from Semen Cassiae.
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Objective To develop a method of quantitative analysis of multi-components by single marker(QAMS) for determination of effective components of naphthopyrone glycosides and anthraquinone aglycone in Cassia tora L.Methods The separation was performed on a Sunfire C18 column (4.6 mm ×250 mm,5 μm), and column temperature 30 ℃.Aetonitrile-0.1% H3PO4 was used as the mobile phase with gradient elution.The detection wavelength was at 278 nm and 284 nm.Relative correction factor by determination of Between aurantio-obtusin and rubrofusarin-gentiobioside or chrysophanol or physcion.the method was evaluated for reproducibility, and the difference between calculated and measured values was compared. Results Rubrofusarin-gentiobioside, aurantio-obtusin, chrysophanol and physcion respectively 0.0503-1.5078, 0.3197-9.5899, 0.5070-15.2108, 0.4027-12.0814μg showed a good linear relationship, and the regression equation is Y =4.95X +2.01(R2 =0.9998),Y =1.03X +0.03(R2 =0.9999),Y=3.98X-0.12(R2 =0.9993),Y =4.81X +0.26(R2 =0.9996).The quantitative results of six batches of Cassia tora L by QAMS was basically consistent with that by external standard method.Conclusion The QAMS method was reliable and accurate, which might be used for the quality control of Cassia tora L.
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Objective: To establish a quantitative analysis of multi-components by single mark (QMSA) for determining the contents of four anthraquinones (aurantio-obtusin, emodin, rhubarb, and physcion) from Cassiae Semen, and verify the feasibility of this method in quality control. Methods: The medicinal material of Cassiae Semen was used as the research object, emodin was used as reference, two kinds of correction methods were used to establish the relative correction factor (fk/s) of aurantio-obtusin, emodin, and physcion. The amount of each component was calculated, at the same time using the external standard method for determination of the three components, comparing the difference between calculated values of QMSA and measured value to validate the feasibility and accuracy of QMSA. Results: The relative correction factors of aurantio-obtusin, emodin, and physcion were established, without significant difference between the calculated values by QMSA and measured values. Conclusion: The experimental QMSA method can accurately determine the contents of the four anthraquinones in Cassiae Semen, and can be used in the multi-index evaluation in Cassiae Semen anthraquinones constituents.
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OBJECTIVE:To establish the HPLC fingerprints for Dangua yangmu cream. METHODS:HPLC was performed on the column of Kromasil C18 with mobile phase of acetonitrile-0.026% phosphoric(gradient elution)at flow rate of 0.8 ml/min,the detection wavelength was 270 nm,the column temperature was 25 ℃ and the injection volume was 20 μl. The chromatographic peak of aurantio-obtusin was used as reference peak to determine the 10 batches of Dangua yangmu cream,and Similarity Evalua-tion System for Chromatographic Fingerprint of TCM(version 2.0)was conducted to identify common peaks and evaluate similari-ty. RESULTS:There were totally 25 common peaks in the 10 batches of Dangua yangmu cream,and the similarity was not lower than 0.921. The validation results showed the fingerprints of 10 batches of Dangua yangmu cream had good consistency with the ref-erence fingerprints. COMCLUSIONS:The established method is specific and reliable,and can provide basis for the quality evalua-tion and control of Dangua yangmu cream.