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Two new compounds, (−)-(6aR,11aR)-4-methoxy-8,9-(methylenedioxy)pterocarpan 3-O-β-D-glucopyranoside (1) and 5-hydroxy-7-methoxyisoflavone 4′-O-β-D-xylopyranosyl-(16)-β-D-glucopyranoside (2), were isolated, together with 30 known compounds from the stems and leaves of Sophora flavescens Aition. Their structures were elucidated by extensive spectroscopic analysis, including HR-ESI-MS data. A preliminary comparison of phenolic metabolite profiles, based on the qualitative HPLC analysis, indicated that the composition of the roots and the aerial parts were significantly different.

The qualitative and quantitative analyses by HPLC and LC-DAD-MS/MS were conducted for the quality consistency evaluation of Compound Kushen Injection (CKI). For fingerprint analysis, 8 peaks were selected as the characteristic peaks in the HPLC chromatograms of 27 different batches of CKI samples and their similarities were more than 0.90, except the four samples. For the typical HPLC profile, peak identification was carried out by HPLC and LC-MS/MS analyses and as a result, 21 chromatographic peaks were identified or characterized based on the comparison of retention time and UV spectra with authentic compounds as well as by summarized MS fragmentation rules. Six of these identified compounds, including oxymatrine, oxysophocarpine, N-methylcytisine, matrine, sophocarpine, and trifolirhizin, were simultaneously determined and the results showed that the total amounts of six marker compounds were variable, to some extent, which was deduced to be related to the quality of the crude materials and the manufac...

Everted intestinal sac models were used to investigate the intestinal absorption of the 4 alkaloids(berberine, palmatine, coptisine, and epiberberine) in Fuzheng Xiaozheng Fang(FZ) at different intestine segments. The absorption parameters of each component were calculated; SPSS 20.0 software was used to analyze the data and evaluate the absorption characteristics at different intestinal segments. The results showed that all the four active ingredients conformed to zero-order absorption rate. There was significant difference in absorption rate constant (Ka) between the four ingredients at low dose and medium and high dose groups(P

The new secoiridoid sulfonates 1–3 were isolated from the 50% EtOH/H2O extract of the sulfiting-processed Lonicera japonica Flos (LJF) by semi-prep. HPLC, and their structures were identified on the basis of mass spectrometry and NMR spectroscopy. HPLC and LC-DAD-MS/MS analyses of the different samples of LJF obtained by various process techniques suggested that the sulfur fumigation led to the decrease of secologanic acid (4) and the formation of secologanic acid-derived sulfonate 1 and its derivatives 2, 2a, and 3 in the crude materials, which revealed that sulfur fumigation, the traditional process technique, could alter the phytochemical profiles of some Chinese herbal medicines.

Simple gas chromatography –mass spectrometry (GC–MS) and highperformance liquid chromatography (HPLC) methods were developed for quantifying eight volatile compounds and 10 sesquiterpenoids, respectively. GC–MS analysis was performed on an HP-5MS capillary column (30 m30.25 mm i.d.) coated with 0.25 mm film 5% phenyl – 95% methylpolysiloxane and selected ion monitoring was used for quantification. Four volatile and previously unquantified monoterpenoids were determined. HPLC analysis was performed on a C18 column with water and acetonitrile as mobile phase. The proposed method, determined 10 non-polar and polar sesquiterpenoids simultaneously, which covered a wider polar range of analytes and had a more perfect resolution. Among them, five sesquiterpenoids were not determined before and some specific components, (4S,5S)germacrone-4,5-epoxide, curcumenone and dehydrocurdione were completely separated for the first time. Both methods were validated for linearity, limit of detection and quantification, precision, accuracy, recovery and system suitability. The methods were simple, effective, reliable and successfully applied to global detection and analysis of volatile and non-volatile components of steamed and non-steamed rhizomes of Curcuma wenyujin (Wen-E-Zhu (WEZ) and Pian-JiangHuang (PJH)). Multivariate statistical analysis was employed to distinguish PJH and WEZ and seven chemical components, including (4S,5S)-germacrone-4,5-epoxide, curcumenone, b-elemene, curzerene, borneol, isoborneol and camphor, were screened as chemical markers. The present study provided a promising method for accurate discrimination of the herbal medicines with the same origin.

The traditional after-harvesting drying method of C. morifolium cv. Hang-ju (HJ) is sun drying, but recently sulfur fumigation is increasingly used as a cheap and convenient method. However, the effects of sulfur fumigation on chemical constituents and potential activities of HJ were unknown. A comprehensively comparison of the chemical profiles between non-fumigated HJ (NHJ) and sulfur-fumigated HJ (SHJ) was conducted by HPLC fingerprints analysis and the discrepant peaks were identified or tentatively assigned by HPLC-ESI/MS(n). Dramatic chemical changes were found that the contents of 4 flavonoid aglycones remarkably increased while those of 7 glycosides significantly reduced which suggested that sulfur-fumigation induced flavonoid glycosides transformed into aglycons by hydrolysis reaction. A significant loss of hydroxycinnamoylquinic acids showed the sulfur fumigation was a destructive effect on HJ. Principal component analysis (PCA) was employed to rapidly discriminate NHJ and SHJ samples. By ICP-OES analysis, it was found that the residue of sulfur of SHJ were three times higher than NHJ (p

Some Curcuma species are widely used as herbal medicines. Sesquiterpenes are their important bioactive compounds and their quantitative analysis is generally accomplished by gas chromatography (GC) or high performance liquid chromatography (HPLC), but the instability and high cost of some sesquiterpene reference standards have limited their application. It is necessary to find a practicable means to control the quality of herbal medicines. Using one stable component contained in Curcuma species to determine multiple analogues should be a practical option. In this study, a simple HPLC method for determination of sesquiterpenes using relative response factors (RRFs) has been developed. The easily available and stable active component curdione was selected as the reference compound for calculating the RRFs of the other eight sesquiterpenes, including zedoarondiol (Zedo), isozedoarondiol (Isoz), aerugidiol (Aeru), (4S,5S)-(+)-germacrone-4,5-epoxide (Epox), curcumenone (Curc), neocurdione (Neoc), germacrone (Germ) and furanodiene (Fura). Their RRFs against curdione were between 0.131-1.301, with a good reproducibility. By using the RRFs, the quantification of sesquiterpenes in Curcuma wenyujin herbal medicines and related products was carried out. The method is especially useful for the determination of (4S,5S)-(+)-germacrone-4,5-epoxide, curcumenone, germacrone and furanodiene, which often are regarded as the principle components in Curcuma species, but unstable when were purified. It is an ideal means to analyze the components for which reference standards are not readily available.

OBJECTIVE: To investigate the effect of different chromatographic conditions on QAMS relative correlation factors (RCF) and relative retention values (RT(R)). METHOD: C18 columns were used with methyl alcohol-0.4% phosphoric acid water (85: 15) as the mobile phase. The detection wavelength was 254 nm, the column temperature was 30 degrees C, and the flow rate was 1.0 mL x min(-1). The five anthraquinones in Rhei Radix et Rhizoma were selected to be the objects of study. The RCF and RT(R) among aloe-emodin, rhein, chrysophanol, physcion and emodin were determined under different chromatographic conditions. RESULT: Their RCFs showed no significant difference. CONCLUSION: The RCFs among anthraquinones established by QAMS can be used as a constant in content determination of traditional Chinese medicines/patent traditional Chinese medicines.

Objective To kinds of establish a HPLC method for determining contents of indole alkaloids and bufadienolides contained in toad medicines, and analyze two kinds of components contained in toad venom, toad skin and toad periostracum. Method As for alkaloids, Nucleosil C18 column was adopted with acetonitrile and water containing 0.5% potassium dihydrogen phosphate (6: 94, adjust pH to 3.2 with phosphate acid) as the mobile phase. The flow rate was 0.8 mL x min(-1), the detection wavelength was 275 nm, and the column temperature was 30 degrees C. As for bufadienolides, Alltima C18 column was adopted with acetonitrile and water containing 0.3% acetic acid (B) as the mobile phase. The gradient process was as follows: a linear gradient from 28% to 54% acetonitrile in the first 15 min, then kept at 54% for additional 20 min. The flow rate was 0.6 mL x min(-1), the detection wavelength was 296 nm, and the column temperature was 30 degrees C. Result The linear ranges were 0.079 6-0.796 microg for serotonin, 0.097 2-1.945 microg for N-methylserotonin, 0.074 4-0.744 microg for N,N-dimethylserotonin, 0.103-2.05 microg for N,N,N-trimethylserotonin, and 0.067 2-0.672 microg for bufothionine, respectively. The average recoveries of serotonin and N-methylserotonin were 98.6% and 91.3%, respectively. The linear ranges of gamabufotalin, bufotalin, bufalin, cinobufagin and resibufogenin were 0.004 83-0.614, 0.007 9-1.006, 0.007 95-1.016, 0.009 7-1.24 and 0.009 6-1.22 microg, respectively, and their average recoveries were 101.6%, 102.5%, 101.0%, 99.1% and 98.9%, respectively. Conclusion Toad venom has the highest contents of indole alkaloids and bufadienolides, followed by toad skin, and toad periostracum showed the lowest contents and even no detection result.

OBJECTIVE To establish a quality evaluation method, quantitative analysis of multi-component with a single-marker (QAMS) to determine the contents of four rhubarb anthraquinones in Sanhuang tablets. METHOD Emodin was used as the internal reference substance, the relative correlation factors (RCF) of rhein, chrysophanol and physcion to emodin were calculated and evaluated. The contents of these four anthraquinones were determined by the external standard method and QAMS, respectively. Rationality, feasibility and repeatability of the QAMS method was verified by comparing the results obtained from the two different methods. RESULT RCFs of rhein, chrysophanol and physcion to emodin against Sanhuang tablets were 1.13, 1.46 and 1.01, respectively, indicating good reproducibilities. The two methods did not show significant difference in results. CONCLUSION The QAMS method can be used a new quality assessment model for quantity of anthraquinones in Sanhuang tablets.

OBJECTIVE To establish a new quantitative method for simultaneous determination of multi-components in Salvia miltiorrhiza by using one chemical reference substance and validate its feasibilities. METHODS The new quality evaluation method, quantitative analysis of multi-components by singer-marker (QAMS), was established and validated with S. miltiorrhiza . Five main ingredients were selected as analytes to evaluate the quatity and their relative correlation factors (RCF) were determined by HPLC-DAD. Within the linear range, the values of RCF at 280 nm of sodium danshensu to protocatechuic aldehyde, rosmarinic acid, lithospermic acid and salvianolic acid B were 7.559, 2.901, 1.825 and 1.746, respectively. The contents of danshensu in the samples of S. miltiorrhiza were determined by using the external standard method, and the contents of the four other ingredients were calculated by their RCFS. The contents of these four ingredients in all samples were also determined by the external standard method. RESULT Within a certain range, the RCFs showed good reproducibility (RSD 1.0%-2.5%). No significant differences were observed between the quantitative results of the two methods. CONCLUSION It is feasible and suitable to evaluate the quality of S. miltiorrhiza and its processed products by QAMS.

Objective To establish a new quantitative method for simultaneous determination of multi-coumarins in Fraxini Cortex by using one chemical reference substance, and validate its feasibilities. Method The new quality evaluation method, quantitative analysis of multi-components by singer-marker (QAMS), was established and validated with Fraxini Cortex. Four main coumarins were selected as analytes to evaluate the quality and their relative correlation factors (RCF) were determined by HPLC-DAD. Within the linear range, the values of RCF at 340 nm of aesculin to asculetin, fraxin and fraxetin were 1.771, 0.799, 1.409, respectively. And the contents of aesculin in samples of Fraxini Cortex were authentically determined by the external standard method, and the contents of the three other coumarins were calculated by their RCF. The contents of these four coumarins in all samples were also determined by the external standard method. Result Within a certain range, the RCF had a good reproducibility (RSD 2.5%-3.9%). Significant differences were not observed between the quantitative results of two methods. Conclusion It is feasible and suitable to evaluate the quality of Fraxini Cortex and its Yinpian by QAMS.

OBJECTIVE: To examine the feasibilities of the method, quantitative analysis of multi-components by single marker (QAMS) for determination of four alkaloids in Xianglian preparations. METHOD: A HPLC method was developed to determine the contents of four alkaloids, epiberberine, coptisine, palmatine and berberine in Xianglian preparations. Berberine was selected as the internal reference substance, and 3 relative correction factors to berberine were calculated. The contents of the four alkaloids in 16 batches of samples were determined by both external standard method and QAMS. The new method was evaluated by comparing the quantitative results with of the external standard method. RESULT: No significant differences were found between the quantitative results of four alkaloids in 16 batches of samples determined by the two methods. CONCLUSION: QAMS is feasible for determination of four alkaloids simultaneously, and the developed method can be used for quality control of Xiang Lian preparations.

OBJECTIVE To remove plumbum ion from the extract of Lonicera japonica by gamma-mercaptopropyl-modified silica gel (MPS). METHOD The reference plumbum ion solution was added into the extract of L. japonica as the tested samples. The static and dynamic adsorptions were investigated to evaluate the influent factors on the removal of plumbum ion in the extract. The solid content and HPLC profiles of the extract were determined to evaluate the process changes. RESULT MPS showed excellent adsorption charateristics to remove plumbum ion from the extract of L. japonica, with fast adsorption rate and more than 80% removal efficiency. The optimum parameters were as follows: 6 times sample volume, 10 times of height to diameter, and 6 BV x h(-1) of flow velocity, at the temperature of 25 degrees C. During the removal process, obvious changes of solid content and HPLC profiles were not observed. CONCLUSION MPS could be used to remove plumbum ion from extract of L. japonica.

OBJECTIVE To study HPLC characteristic fingerprint of Moghania philippinensis and provide a reliable method for scientific evaluation and quality control. METHOD The chromatographic separation was performed on a Kromasil C15 column (4.6 mm x 250 mm, 5 microm). The mobile phase consisted of acetonitrile and water containing 0.3% acetic acid in gradient elution. The column temperature was set at 40 degrees C and the detection wavelength was at 254 nm. RESULT The developed HPLC fingerprint method above was applied to analyze 23 batches of crude herbs of Moghania philippinensis. The total 22 peaks were selected as the characteristic peaks. And five of them were identified as genistein, genistin, 5,7,3',4'-tetrahydroxy-6,8-diprenylisoflavone, 5,7,4'-trihydroxy-6,8-diprenylisoflavone and flemiphilippinin E by matching their retention time, UV spectra data with those of the authentic chemical reference substances. CONCLUSION The method is simple, accurate and reproducible. It is suitable for the quality control of M. philippinensis.

OBJECTIVE To study the key processes of Fufang Kushen injection for technical upgrading. METHOD Total alkaloids (sum of matrine, oxymatrine, sophoridine and oxysophoridine) and macrozamin were selected as quality evaluation markers. The key processes of percolation with acetic acid and discoloration with activated carbon were optimized by orthogonal experiment design, and process of purification with alcohol was investigated by single factor method. RESULT The optimal condition of percolation process is as follows: the medicinal materials are soaked for 9 h with 4 times water containing 0.8% acetic acid, then percolation starts at flow-rate of 5 mL x min(-1) x kg(-1) and adding 2 times 0.8% acetic acid solution is added at the same velocity. Purification process is that the concentrated solution is precipitated by 60%, 80% and 90% alcohol in turn. Discoloration process is that 6 activated carbon is added into the solution which is heated at 60 degrees C for 20 minutes. CONCLUSION The optimal extraction process is not only simple, saving the industrial cycle, reducing the potential risk, but also decreasing the acetic acid amount to guarantee the acid-insoluble ash as well as the functional ingredients.

A HPLC method for limit detection of aristolochic acid A in the Chinese herbs containing aristolochic acid or suspected-containing aristolochic acid and their preparations was established. The samples were analyzed on an Alltima C18 column eluted with methanol-water-acetic acid (68:32:1.5) as the mobile phase. Flow rate was at 1.0 mL x min(-1) and the detection wavelength was at 390 nm. The calibration curve was linear over the range from 0.016 to 0.51 g (r = 0.9993) and LOD was 4 ng. The average recovery was 101.2% with RSD of 2.01%. The procedures of sample preparation were systematically investigated. The contents of aristolochic acid A in Radix et Rhizoma Asari bought from market or drugstore were fluctuated from 3.1 to 26.6 microg x g(-1) and 3 of 11 samples accorded with the quality requirement of current Chinese Pharmacopoeia. Among 15 batches samples of Chinese medicaments, only one sample was found to contain aristolochic acid A. The present investigation shows that the method is sensitive and repeatable and it could be used for the limit detection of aristolochic acid A in the Chinese herbal medicines containing trace amount of aristolochic acid A or suspected-containing aristolochic acid A and their preparations.

OBJECTIVE To develop a GC-MS method for the determination of methyl nonyl ketone in the volatile oil from the herbs of Houttuynia cordata. METHOD The sample was split in the 240 degrees C injection port, with 20:1 split ratio, and separated on a DB-5 (30 m x 0.25 mm, 0.25 microm film thickness) fused silica column with helium as the carrier gas. The temperature program was as follows: 100 degrees C for 2 min, the 5 degrees C x min(-1) to 150 degrees C, then 15 degrees C x min(-1) to 200 degrees C, and kept for 10 min. The MS transfer line temperature was set to 250 degrees C, the MS source temperature was set to 200 degrees C. The ionization mode was electron ionization (EI) and the selective ion monitor mode was used. RESULT A good linear relationship was constructed over the injection amount range of 5.5-110 ng of methyl nonyl ketone. The average recovery was 98.9%, and RSD was 2. 2%. CONCLUSION The developed method was sensitive, accurate, and can be used for the determination of methyl nonyl ketone in the volatile oil and for the quality control of H. cordata.

Objective To establish a method for quick finding the absorption ingredients of Wuzhuyu decoction in order to select the index to control its quality. Method The absorption of three concentration of Wuzhuyu decotion was investigated with the in vitro-everted intestinal sac model. The intestinal bag fluid of jejunum and ileum were collected in different time and the eight ingredients, which were evodiamine (Ev), rutaecarpine (Ru), limonin (Li), ginsenoside-Rb1, -Rg1, -Re (Rb1, Rg1, Re), isorhamnetin-3-O-beta-D-glucosyl(6''-->1'")-alpha-L-rhamnoside (Irs)and 6-gingerol (6-Gi), were detected by HPLC as the represent constituents in samples. Result Eight ingredients except Ru in samples could be detected, but Ev could not be detected in high concentration samples. The ratios between absorption ingredients were different from in Wuzhuyu decotion. Conclusion The in vitro-everted intestinal sac canc absorb the ingredients of Wuzhuyu decotion selectivity. Compare with the ileum, the jejunum can provide the more absorption information and faster, the best test time is 60-90 min.

Abroad review of current methods for the recovery of liquid residual accelerants in fire debris is given. A summary of current practices of sample preparation methods in U.S. laboratories is presented. Sampling of heated headspace is useful as a screening method. It is also applicable for samples that contain a high concentration of accelerant. Distillation-based methods are effective only when large amounts of accelerants are present but they permit the physical isolation of relatively pure liquids, including some water-soluble materials such as alcohols. Solvent extraction is particularly advantageous for accelerants of low volatility such as diesel fuel or highly evaporated petroleum-based products, but it is very susceptible to interferences from the matrix. Dynamic enrichment by adsorption/elution is the most popular and widely used recovery method for liquid accelerants. It offers high enrichment factors but shows weaknesses with respect to polar and low-volatility liquids. No single method is universally effective for all types of accelerants that are commonly encountered in practice. It appears that currently applied recovery methods are particularly weak for water-soluble organics such as alcohols. Sample preparation methods have to be viewed in conjunction with the method to be used to characterize and identify suspect accelerants. Gas chromatography is used almost exclusively for separation and measurement. Selective detection of components that are diagnostic of accelerants allows important trade-offs between sensitivity, chromatographic efficiency and the level of interferences that can be tolerated. Pattern recognition with comparison of chromatographic profiles is greatly simplified if interferences from the matrix can be suppressed. Application of capillary columns capable of high resolution facilitates the recognition of diagnostically important components. Petroleum-based fluids and products are ubiquitous in the human environment and it is therefore particularly important to pay attention to petroleum-based fluids that are derived from such sources. Many common inconspicuous household materials contain petroleum-based solvents and are thus a part of the natural background. The term sensitivity as it relates to the effectiveness of a recovery method must be critically viewed in this light.