Comparison of microwave‐assisted and heat reflux extraction techniques for the extraction of ten major compounds from Zibu Piyin Recipe using ultra high performance liquid chromatography with tandem mass spectrometry
Abstract:Microwave-assisted extraction and efficient ultra-high performance liquid chromatography with triple quadrupole mass spectrometry were previously used to quickly extract and simultaneously quantify ginsenoside Rf, Ro, and Rd, 20(S)-ginsenoside-Rg2 , 20(R)-ginsenoside-Rg2 , tanshinone IIA, cryptotanshinone, dihydrotanshinone I, lithospermic acid, and osthole from Zibu Piyin Recipe. We here showed that heat reflux extraction provides higher extraction efficiency of these target compounds but is more time consumi… Show more
“…And the content variation degrees for the different structural types of compounds were gingerols > flavonoids > aromatic acids > alkaloids > phthalides, which might be related to the pharmacological function of XSHG. Compared with some studies on the content changes of main components in TCM formulae after compatibility , the majority of bioactive components in XSHG increased at different degrees, which indicated the XSHG preparation was a reasonable prescription and provided a scientific basis for the wide use of XSHG in clinical practice. And the main causes of these results were analyzed as follows.…”
Section: Discussionmentioning
confidence: 77%
“…Other chemicals and reagents were analytical grade. Chemical standards including trigonelline (1), stachydrine hydrochloride (2), thymine (3), protocatechuic acid (4), hydroxysafflor yellow A (5), chlorogenic acid (6), amygdalin (7), caffeic acid (8), leonurine hydrochloride (9), rutin (10), p-coumaric acid (11), liquiritin (12), ferulic acid (13), kaempferol-3-O--D-rutinoside (14), zingerone (15), isoliquiritoside (16), senkyunolide I (17), senkyunolide H (18), liquiritigenin (19), quercetin (20), kaempferol (21), glycyrrhizic acid (22), 6-gingerol (23), senkyunolide A (24), ligustilide (25), butylidenephthalide (26), and 6-shogaol (27) were all obtained from Sichuan Shinning Biotech Institute (Chengdu, China). The purity of each reference compound was over 98%, as determined by HPLC with peak area normalization method.…”
Xin-Sheng-Hua granule, a representative formula for postpartum hemorrhage, has been used clinically to treat postpartum diseases. Its main bioactive components comprise aromatic acids, phthalides, alkaloids, flavonoids, and gingerols among others. To investigate the changes in main bioactive constituents in its seven single herbs before and after compatibility, a rapid, simple, and sensitive method was developed for comparative analysis of 27 main bioactive components by using ultrahigh-performance liquid chromatography with triple quadrupole electrospray tandem mass spectrometry for the first time. The sufficient separation of 27 target constituents was achieved on a Thermo Scientific Hypersil GOLD column (100 mm × 3 mm, 1.9 μm) within 20 min under the optimized chromatographic conditions. Compared with the theoretical content, the observed content of each analyte showed remarkable differences in Xin-Sheng-Hua granule except thymine, p-coumaric acid, senkyunolide I, senkyunolide H, and ligustilide; the total contents of 27 components increased significantly, and the content variation degrees for the different components were gingerols > flavonoids > aromatic acids > alkaloids > phthalides. The results could provide a good reference for the quality control of Xin-Sheng-Hua granule and might be helpful to interpret the drug interactions based on variation of bioactive components in formulae.
“…And the content variation degrees for the different structural types of compounds were gingerols > flavonoids > aromatic acids > alkaloids > phthalides, which might be related to the pharmacological function of XSHG. Compared with some studies on the content changes of main components in TCM formulae after compatibility , the majority of bioactive components in XSHG increased at different degrees, which indicated the XSHG preparation was a reasonable prescription and provided a scientific basis for the wide use of XSHG in clinical practice. And the main causes of these results were analyzed as follows.…”
Section: Discussionmentioning
confidence: 77%
“…Other chemicals and reagents were analytical grade. Chemical standards including trigonelline (1), stachydrine hydrochloride (2), thymine (3), protocatechuic acid (4), hydroxysafflor yellow A (5), chlorogenic acid (6), amygdalin (7), caffeic acid (8), leonurine hydrochloride (9), rutin (10), p-coumaric acid (11), liquiritin (12), ferulic acid (13), kaempferol-3-O--D-rutinoside (14), zingerone (15), isoliquiritoside (16), senkyunolide I (17), senkyunolide H (18), liquiritigenin (19), quercetin (20), kaempferol (21), glycyrrhizic acid (22), 6-gingerol (23), senkyunolide A (24), ligustilide (25), butylidenephthalide (26), and 6-shogaol (27) were all obtained from Sichuan Shinning Biotech Institute (Chengdu, China). The purity of each reference compound was over 98%, as determined by HPLC with peak area normalization method.…”
Xin-Sheng-Hua granule, a representative formula for postpartum hemorrhage, has been used clinically to treat postpartum diseases. Its main bioactive components comprise aromatic acids, phthalides, alkaloids, flavonoids, and gingerols among others. To investigate the changes in main bioactive constituents in its seven single herbs before and after compatibility, a rapid, simple, and sensitive method was developed for comparative analysis of 27 main bioactive components by using ultrahigh-performance liquid chromatography with triple quadrupole electrospray tandem mass spectrometry for the first time. The sufficient separation of 27 target constituents was achieved on a Thermo Scientific Hypersil GOLD column (100 mm × 3 mm, 1.9 μm) within 20 min under the optimized chromatographic conditions. Compared with the theoretical content, the observed content of each analyte showed remarkable differences in Xin-Sheng-Hua granule except thymine, p-coumaric acid, senkyunolide I, senkyunolide H, and ligustilide; the total contents of 27 components increased significantly, and the content variation degrees for the different components were gingerols > flavonoids > aromatic acids > alkaloids > phthalides. The results could provide a good reference for the quality control of Xin-Sheng-Hua granule and might be helpful to interpret the drug interactions based on variation of bioactive components in formulae.
“…As summarised in Table , the sensitivity of the developed method was 22–124 times greater than those of HPLC‐UV methods, 5–37 times greater than those of HPLC‐ECD methods, 15–17 times greater than those of the LC–MS method, 5.5–26 times higher than those of the LC‐Q‐TOF‐MS method and 2–3.4 times higher than those of the LC–MS/MS method reported by Xu et al . (). Although the proposed method was less sensitive when compared to the LC–MS/MS method reported by Zhang et al .…”
Section: Resultsmentioning
confidence: 97%
“…Many chromatographic methods have been described for simultaneous assay of tanshinones: micellar electrokinetic chromatography with ultraviolet (UV) detection (Cao et al ., ), high‐performance liquid chromatography (HPLC) with UV detection (Chang et al ., ; Wang et al ., ; Wang et al ., ), electrochemical detection (ECD) (Chen et al ., , ) and LC with mass spectrometry either with electrospray ionisation mass spectrometry (LC‐ESI‐MS) (Chen et al ., ), LC with tandem mass spectrometry (LC–MS/MS) (Xu et al ., ; Zhang et al ., ) or LC with quadrupole time‐of‐flight tandem mass spectrometry (LC‐Q‐TOF‐MS/MS) (Zhou et al ., ). However, HPLC‐UV methods do not have adequate selectivity and sensitivity to detect trace levels of tanshinones.…”
ABSTRACT:Introduction -Tanshinones are a major class of bioactive ingredients in the traditional herbal medicines, Danshen (Salvia miltiorrhiza). A sensitive and reliable determination method for tanshinones is useful to ensure the quality of Danshen. Objective -To develop a sensitive and selective analytical method for tanshinones by high-performance liquid chromatography (HPLC) with fluorescence detection after pre-column derivatisation. Methodology -The proposed method depends on derivatisation reaction of tanshinones with 4-carbomethoxybenzaldehyde and ammonium acetate forming intensely fluorescent imidazole derivative. Results -The proposed method provided excellent sensitivity with the detection limits of 3.3 nM (66 fmol/injection), 3.2 nM (64 fmol/injection) and 2.0 nM (40 fmol/injection) for cryptotanshinone, tanshinone I and tanshinone IIA, respectively, without the necessity of complicated instrumentations. The developed method is successfully applied to quantify the contents of tanshinones in Danshen. Conclusion -The developed method is the first analytical method for tanshinones by fluorescence detection. Since the derivatisation reaction is selective for the o-quinone structure of tanshinone, the developed method will become a suitable mean for the discovering of tanshinone type diterpenoids from herbal samples.
“…To achieve rapid determination of multiple alkaloids in Corydalis decumbens, sample preparation is a crucial step. MAE has become a widely used technique for the extraction of bioactive constituents in natural products as reported extensively in the literatures [21][22][23][24][25][26]. Microwaves can pass into the plant tissues and rapidly produce heat to break cells.…”
A rapid and cost-effective method based on microwave-assisted extraction followed by capillary electrophoresis was developed for simultaneous quantification of seven alkaloids in Corydalis decumbens for the first time. The main parameters affecting microwave-assisted extraction and capillary electrophoresis separation were investigated and optimized. The optimal microwave-assisted extraction was performed at 40°C for 5 min using methanol/water (90:10, v/v) as the extracting solvent. Electrophoretic separation was achieved within 15 min using an uncoated fused-silica capillary (50 μm internal diameter and 27.7 cm effective length) and a 500 mM Tris buffer containing 45% v/v methanol (titrated to pH 2.86 with H PO ). The developed method was successfully applied to the quantification of seven alkaloids in Corydalis decumbens obtained from different regions of China. The combination of microwave-assisted extraction with capillary electrophoresis was an effective method for the rapid analysis of the alkaloids in Corydalis decumbens.
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