To establish a fingerprint spectrum for Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran based on UFLC/Q-TOF-MS, and make a principal component analysis (PCA) with Markview software, in order to compare the changes of components between raw and processed Atractylodis Macrocephalae Rhizoma with raw wheat bran as the blank. The results showed that the changed in components raw Atractylodis Macrocephalae Rhizoma and Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran were apparently observed by PCA. Six compounds were identified to have significant changes in mass fraction before and after being stir-fried, namely atractylenolide-I, atractylenolide-II, atractylenolide-III, atractylentrid, atractylon and an unknown compound. Among them, atractylenolide-I and atractylenolide-II generated from dehydration and dehydrogenation of atractylenolide-III may be the material base of Atractylodis Macrocephalae Rhizoma stir-fried with wheat bran for strengthening spleen.
Atractylodes ; chemistry ; Chromatography, Liquid ; methods ; Dietary Fiber ; Lactones ; analysis ; Mass Spectrometry ; Principal Component Analysis ; Sesquiterpenes ; analysis

OBJECTIVETo develop an HPLC method for simultaneous determination of three major sesquiterpene lactones in Radix Linderae.

METHODThe chromatographic separation was achieved on a Diamonsil C18 column (4.6 mm x 250 mm, 5 microm) using isocratic elution of acetonitrile-water (containing 0.1% H3 PO4) (45 : 55) at a flow rate of 1.0 mL x min(-1). Detection was carried out using a photodiode array detector at 220 nm.

RESULTThe calibration curves were linear in the range of 0.001 8-0.036 0 g x L(-1) for hydroxylinderstrenolide (R2 = 0.999 8), 0.016 2-0.323 2 g x L(-1) for neolinderalactone (R2 = 0.999 9), 0.010 5-0.209 9 g x L(-1) for linderane (R2 = 0.999 9), respectively. The average recoveries were 100.0% for hydroxylinderstrenolide, 98.8% for neolinderalactone and 98.9% for linderane with RSD not more than 3.3%.

CONCLUSIONThe established method was proved to be simple, sensitive and credible, and can be applied to quality control of Radix Linderae.

Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; Lactones ; analysis ; Lindera ; chemistry ; Sesquiterpenes ; analysis

An HPLC method was established to simultaneously determine the five sesquiterpene lactones, carabrone, carabrol, 2-desoxy-4-epi-pulchellin, telekinand 11(13)-dehydroivaxillin in Carpesium abrotanoides. Samples were analyzed on a kromasil C18 column (4.6 mm x 250 mm, 5 µm); mobile phase: A was acetonitrile, B was water, with gradient elution; flow speed: 1.0 mL · min(-1); detection was carried out using a photodiode array detector at 211 nm; temperatureof column: 30 °C. The five sesquiterpene lactones were well separated with good linear correlations in the range of 0.270-2.700 (r = 0.999 7 ), 1.336-13.360 (r = 0.999 6), 0.258-2.580 (r = 0.999 7), 0.238-2.380 (r = 0.999 9), 0.490-4.900 µg (r = 0.999 9) for carabrone, carabrol, 2-desoxy-4-epi-pulchellin, telekin and 11 (13) -dehydroivaxillin. The average recoveries of these five sesquiterpene lactoneswere 96.78%-98.41% (RSD 1.3%-2.9%). The method was simple, repeatable and stable, which could be used for quality control of C. abrotanoide.
Asteraceae ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; Lactones ; analysis ; Sesquiterpenes ; analysis

In order to study the correlation between the traits of Andrographis paniculata. The main agronomic traits and the content of four kinds of diterpene lactons were measured by the seedlings and the unmutagenized seeds carried by the spacecraft,and multiple comparisons,correlations and principal component analysis were carried out. The results showed that the agronomic traits of A. paniculata have different degrees of difference after being carried by space. The contents of diterpene lactones were quite different. The variation coefficients of deoxyandrographolide content,fresh weight,leaf dry weight,dehydrated andrographolide content,dry weight,neoandrographolide content and andrographolide content were all over 35%. There was a significant correlation between multiple traits,and the leaf weight ratio was significantly positively correlated with the number of primary tillers,leaf dry weight and dry weight,and was significantly negatively correlated with the content of deoxyandrographolide. Andrographolide content was a significantly negatively correlated with the number of leaves and the number of primary tillers,and positively correlated with the other three lactones. Five principal components were extracted from principal component analysis,and the cumulative contribution rate was 83. 127%,which were yield factor,plant type factor,leaf type factor,component factor and seed weight factor. Among the traits affecting the quality of A. paniculata,the yield factor for reliability of the selection of A. paniculata is higher than other factors. There are abundant variations among the traits of A. paniculata,carried in space which increase the genetic diversity. The principal component analysis method can be used to select the principal component factors according to the breeding requirements,which provides a theoretical basis for the breeding of high-yield and high-quality A. paniculata and the high-yield and stable cultivation of A. paniculata.
Andrographis ; chemistry ; Diterpenes ; analysis ; Lactones ; analysis ; Phytochemicals ; analysis ; Plant Leaves ; Reproducibility of Results

OBJECTIVETo screen the potential hepatotoxic components in Chinese herb medicine Aucklandiae Radix.

METHODSThe potential hepatotoxic components were screened using HepG2 cells labeled with fluorescein diacetate from 25 fractions of Aucklandiae Radix, in which the hepatotoxic compounds were further identified with GC-MS.

RESULTSTen potential hepatotoxic fractions were screened. The identification results by GC-MS indicated that the main compounds in C09 were dehydrocostuslactone, santamarine (or magnolialide) and reynosin, and in C11 were α-costol and elemol.

CONCLUSIONDehydrocostuslactone, santamarine (or magnolialide), reynosin, α-costol and elemol are potential hepatotoxic compounds in Aucklandiae Radix.

Drugs, Chinese Herbal ; chemistry ; Gas Chromatography-Mass Spectrometry ; methods ; Lactones ; analysis ; toxicity ; Sesquiterpenes ; analysis ; toxicity

OBJECTIVETo develop an UPLC-MS method for the simultaneously quantitation of adonifoline and senecinine in Senecio herbs.

METHODUPLC-Micro 2000 was used for quantification in SIR mode under ESI+. Monocrotaline was used as the internal standard. Chromatography was performed on a Shiseido Capcell Pak MG (2.0 mm x 50 mm, 3 microm) column at 30 degrees C using an gradient elution of acetonitrile-0.5% formic acid in water at the flow rate of 0.3 mL x min(-1). The injection volume was 2 microL.

RESULTGood linearity was obtained for quantitation of adonifoline over the range of 1.02-816.00 microg x L(-1) (r = 0.998 0). And recoveries at different concentration levels were between 95.73% and 103.0% with RSDs no more than 2.5%. For quantification of senecionine, the linear range was between 1.08-860.56 microg x L(-1) (r = 0.997 6). And recoveries at different concentration levels were between 95.67% and 101.5% with RSDs no more than 2.3%. Good reproducibility and precision were also achieved.

CONCLUSIONThe new developed UPLC method is sensitive, accurate and reliable enough for the quantitation of adonifoline and senecionine in Senecio herbs thus can be used for the limit detection of pyrrolizidne alkaloids in S. scandens. It can also be used for the identification of fake drugs of S. scandens such as S. vulgaris. The developed method was served for the quality evaluation of Herba Senecionis Scandentis.

Chromatography, Liquid ; methods ; Lactones ; analysis ; Mass Spectrometry ; methods ; Pyrrolizidine Alkaloids ; analysis ; Senecio ; chemistry

OBJECTIVEA RP-HPLC method was developed for simultaneous determination of bigelovin, ergolide and tomentosin in Inula hupehensis.

METHODAn Agilent C18 column (4.6 mm x 250 mm, 5 microm) was used for separation at 40 degrees C. The mobile phase was acetonitrile-water, and the flow rate was 1.2 mL x min(-1). The detection wavelength was set at 210 nm.

RESULTThe method has good linearity in the ranges of 0.01792-0.1792 g x L(-1) (r =0.9999) for bigelovin, 0.0424-0.4240 g x L(-1) (r =0.9996) for ergolide, and 0.044 8-0.4480 g x L(-1) (r = 0.9996) for tomentosin. The average recoveries of bigelovin, ergolide, and tomentosin were 98.5%, 98.2%, 98.4%, with the RSD of 1. 3%, 1.3%, 1.7%, respectively. The results demonstrated that there was a significant difference in the contents of three sequterpene lactones among the tested Inulae Flos.

CONCLUSIONThe results indicated that the present RP-HPLC method is simple, quick and accurate, and can be used for the quality control of I. hupehensis, especially for the authentication of Inulae Flos.

Chromatography, High Pressure Liquid ; methods ; Inula ; chemistry ; metabolism ; Lactones ; analysis ; Sesquiterpenes ; analysis

This study established a method for rapid quantification of terpene lactone, bilobalide, ginkgolide C, ginkgolide A and ginkgolide B in the chromatographic process of Ginkgo Folium based on near infrared spectroscopy(NIRS). The effects of competitive adaptive reweighting sampling(CARS), random frog(RF), and synergy interval partial least squares(siPLS) on the performance of partial least squares regression(PLSR) model were compared to the reference values measured by HPLC. Among them, the correlation coefficients of prediction(Rp) of validation sets of terpene lactone, bilobalide, and ginkgolide C were all higher than 0.98, and the relative standard errors of prediction(RSEPs) were 5.87%, 6.90% and 6.63%, respectively. Aiming at ginkgolide A and ginkgolide B with relatively low content, the genetic algorithm joint extreme learning machine(GA-ELM) was used to establish the optimized quantitative analysis model. Compared with CARS-PLSR model, the CARS-GA-ELM models of ginkgolide A and ginkgolide B exhibited a reduction in RSEP from 15.65% to 8.52% and from 21.28% to 10.84%, respectively, which met the needs of quantitative ana-lysis. It has been proved that NIRS can be used for the rapid detection of various lactone components in the chromatographic process of Ginkgo Folium.
Chromatography, High Pressure Liquid ; Ginkgo biloba ; Lactones/analysis* ; Least-Squares Analysis ; Spectroscopy, Near-Infrared/methods*

OBJECTIVETo investigate the sesquiterpene lactones of the aerial parts of Inula helianthus-aquatica.

METHODCompounds were isolated and purified by silica gel, Sephadex LH-20 and preparative HPLC. On the basis of physicochemical properties and spectroscopic data, their structures were identified.

RESULTSeven sesquiterpene lactones and four other compounds were obtained and identified as 2-desoxy-4-epi-pulchellin (1), 6-acetoxy-4-hydroxy-1, 10H-pseudoguaia-11 (13)-en-12,8-olide (2), 4-acetoxy-6-hydroxy-1, 10H-pseudoguaia-11(13)-en-12,8-olide (3), 8-epi-inuviscolide (4), 2,3,11,13-tetrahydroaromaticin (5), 11,13-dihydro-ergolide (6), 4-epipulchellin-2-O-acetate (7), 7-epiloliolide (8), loliolide (9), beta-sitosterol (10) and daucosterol (11).

CONCLUSIONAll the compounds were isolated from this plant for the first time.

Drugs, Chinese Herbal ; chemistry ; Inula ; chemistry ; Lactones ; analysis ; chemistry ; isolation & purification ; Sesquiterpenes ; chemistry

To provide supports for Ginkgo biloba cell engineering for production of Terpene lactones (Ginkgolides and bilobalide), the cell suspension were established from calli induced from zygote embryos and stems of 30-day-old seedlings respectively. The relationship between cell growth, differentiation and the terpene lactone accumulation in these suspension cultures were investigated. HPLC determination indicated that, the ginkgolide B was found in the embryo derived cell suspension cultures at 0.044% of cell dry weight, and this result was the first time reported in this study. The accumulation of terpene lactone in the suspension cultures derived from both the embryo and seedling stems are effected by the level of the cell differentiation. The ginkgolide B was only found in small cell aggregates in the size smaller than 2mm, and the highest level of ginkgolide B was accumulated in cell aggregates in the size smaller than 1mm; however, the cell aggregates in the size bigger than 3mm could only produced bilobalide and ginkgolide A. In the same size aggregates of the suspension cultures the terpene lactone accumulation is strongly effected by the source of the explant. When the size of cell aggregates was in less than 1mm, the concentration of bilobalide, ginkgolide A and B in the cell suspension cultures derived from the embryos was 2, 1.4 and 0.56-fold, respectively, higher than that of cell cultures derived from seedling stems.
Bilobalides ; analysis ; Cell Differentiation ; physiology ; Cell Proliferation ; Culture Techniques ; methods ; Ginkgo biloba ; growth & development ; metabolism ; Ginkgolides ; analysis ; Lactones ; analysis