ABSTRACT
n-Octanol/ water partition coefficients (Kow ) is an important parameter commonly used to explain toxicity, activity and transmembrane of drugs. However, it is difficult to be detected by direct experimental determination. In this work, a set of 29 neutral and acidic analogues of naphthalene and anthraquinone with reliable experimental Kow data was chosen as model compounds for establishing linear relationship between the logarithm of apparent n-octanol/ water partition coefficient (lgKow), and the logarithm of reversed phase-high performance liquid chromatography (RP-HPLC) retention factor of the solutes corresponding to neat aqueous fraction of mobile phase (lgkw ) as the quantitative structure-retention relationship (QSRR) model. Methanol-water mixture was used as mobile phase at various pH, and retention time (tR ) was rectified by a dual-point retention time correction (DP-RTC) in this method. The experiment results indicated that the proposed QSRR model had good correlation coefficient R2 = 0. 974 -0. 976 with satisfactory results of internal and external validation (the cross-validated correlation coefficient R2cv of 0. 970-0. 973, and 1. 4% ≤relative error (RE)≤7. 9% for all the 6 verification compounds). In addition, this QSRR model was compared with linear solvation energy relationship ( LSER) involved in different descriptors of molecular structure, showing no differences. The QSRR model was applied to measure Kow of 11 naphthalenes and anthraquinones, and the predicted data were compared with Shake-flask method (SFM) experimental ones, as well as calculated ones obtained by software. The results suggested that the proposed method for Kow determination in this work was more accurate, simple and fast. To the best of our knowledge, this is the first report on measuring Kow data for these compounds. The proposed strategy provides the possibility in determining Kow of lipophilic components in complex mixture more quickly and accurately by RP-HPLC.
ABSTRACT
The fingerprint chromatograms of Arisaematis Rhizoma were established by HPLC. The analysis was performed on a Lichrospher C18 (4.6 mm x 200 mm, 5 microm) column with acetonitrile-water (containing 0.1% acetic acid) as mobile phase at a flow rate of 1.0 mL x min(-1). The detection wavelength was set at 270 nm, and the column temperature was 30 degrees C. The similarities of the fingerprint chromatograms were calculated over 0.9 between 11 batches of Arisaematis Rhizoma samples by analyzing 14 common peaks with adenosine as reference substance. However, their fingerprint chromatograms were significantly different from those of Pinellia pedatisecta and P. ternate. Adenine, hypoxanthine, xanthine, uridine, guanosine, adenosine, schaftoside, and isoschaftoside were identified by comparing the retention times and their ultraviolet spectra. The method is repeatable, exclusive and can be used for identification and evaluation of Arisaematis Rhizoma.
Subject(s)
Arisaema , Chemistry , Chromatography , Drugs, Chinese Herbal , Chemistry , Reference Standards , Quality Control , Reproducibility of ResultsABSTRACT
<p><b>OBJECTIVE</b>To investigate the flavonoids in Platycladi Cacumen.</p><p><b>METHOD</b>The constituents in Platycladi Cacumen were determined by UPLC-MS. A Waters BEH C18 column (2.1 mm x 150 mm, 1.7 microm) was used with a gradient elution of methanol-water containing 0.2% formic acid. The mass spectrometer equipped with electrospay ionization source was used as defector and operated in data was collected under the negative ion modes.</p><p><b>RESULT</b>Eleven constituents were identified.</p><p><b>CONCLUSION</b>In this study, the main flavonoids in Platycladi Cacumen were separated by UPLC, and identified through the information of mass number and UV spectra. With the information of MS/MS from flavonoids, the modes of breaking up flavonoids were discussed. It is an accurate and effective method which can be applied for the constituent identification of Platycladi Cacumen.</p>
Subject(s)
Chromatography, Liquid , Methods , Cupressaceae , Chemistry , Flavonoids , Chemistry , Mass Spectrometry , Methods , Plant Extracts , ChemistryABSTRACT
Objective To study the effects of caesarean section on breastfeeding.Methods Divides into 2 groups stochastically 120 example c-section parturient woman,each group of 60 examples,the control group gives obstetrics conventional nursing;The observation group carries on the target-oriented behavior intervention and psychological unblocking by professional nurse to the parturient woman:Uses the pre-natal health education seepage,instructs the parturient woman to feed correctly nurses the skill,promotes the wet-nurse nutrition,dredges intervention measures promptly and so on mammary gland tube.Results The observation group parturient women compare the control group to secrete young timing advance,secrete the young quantity to increase,the early nursing success ratio is high,the difference has the significance (P<0.01).Conclusion Early interventions to parturient after caesarean section is propitious to their health recover and elevate the success rate of early breast feeding.
ABSTRACT
OBJECTIVE:To identify the medical material Ranunculus ternatus. METHODS: Potassium bromide was used for tabletting.The medical material Ranunculus ternatus and its isogeneric plants were analyzed by using infrared spectrometry.RESULTS:The infrared spectrogram of the medical material Ranunculus ternatus was distinctive and somewhat different from those of its isogeneric plants.CONCLUSION:Fourier transformation infrared spectrometry could be used for the identification of Ranunculus ternatus in that it is simple,rapid,reproducible and specific.
ABSTRACT
OBJECTIVE:To establish the identification method of Rhizoma Arisaematis and content determination of flavon-oids.METHODS:TLC was used to identify Rhizoma Arisaematis with schaftoside and ischaftoside as reference substances.The content of flavonoids was determined by HPLC.RESULTS:TLC of test sample and that of control substance had same color dots.The linear range of schaftoside and isoschaftoside were 7.925～126.8 ?g?mL-1(r=0.999 9) and 3.996～63.94 ?g?mL-1(r=0.999 7) respectively.Average recoveries were 99.4% for schaftoside (RSD=2.10%,n=9) and 99.52% for isoschaftoside(RSD=2.42%,n=9).CONCLUSION:The method is simple,accurate and reproducible for the quality evaluation of Rhizoma Arisaematis.
ABSTRACT
OBJECTIVE To establish a HPLC-RI assay for the determination of astragaloside IV in the Huangqijing solution.METHODS The column Hypersil ODS 2(4.6 mm×200 mm,5 μm) was used.The mobile phase was consisted of methanol ane water (67∶33).The flow rate was 1 mL.min-1.RESULTS The standard curve was linear over the range of 1～5 μg with the correlation coefficient 0.9999.The average recovery was 98.1% with the RSD 2.02%(n＝6).CONCLUSION This method was sensitive,accurate,repeatable and easy to operate.
ABSTRACT
AIM: To establish a sensitive and specific liquid chromatobraphy-mass spectrometry(time-of-flight)[LC-MS(TOF)] for the determination of astragaloside Ⅳ in rabbit plasma. METHODS: The HPLC-MS utilizing solid phase extraction was established to determine the concentration of astragaloside IV and ginsenoside R_~g1 , was used as internal standard. The analysis was carried on Agilent Hypersiol ODS(5 ?m, 4.6 mm?250 mm) column with a mobile phase of methanol-water (80∶20, v/v).Detection was performed on a time-of-flight mass spectrometry equipped with an ESI internal and operated in positive-ionization mode. Astragaloside Ⅳ quantitation was realized by computing the peak area ratio (astragaloside Ⅳ-ginsenoside R_~g1 )(astragaloside Ⅳ m/z807[M+Na]+ and ginsenoside R_~g1 m/z823[M+Na]+) and comparing them with calibration curve (r=~0.999 ). RESULTS: The linear calibration curve was obtained in the concentration range of 0.01-5 ?g?L~-1 .The detection limit of astragaloside Ⅳ was 0.01 ?g?L~-1 .The average recovery was more than 98%.The intra-and inter-run precision was measured to be below 5% of RSD. CONCLUSION: The method is sensitive, simple and rapid ,so, it can meet the need for the pharmacokinetics and bioavailability of astragaloside Ⅳ.
ABSTRACT
AIM: To establish a HPLC for determination of puerarin and baicalin in Gegen Qinlian Micropill. METHODS: A Kromasil C 18 Column was used. The mobile phase was methanol-0.2% phosphoric acid. Puerarin and baicalin were determined by dual wavelength, ? 1=250nm. ? 2=315nm. RESULTS: The linear range of puerarin was within 32.0 ng—288.0 ng,r=0.9998 and the sample recovery was 100.17 % (RSD=1.00%(n=9)). The linear range of baicalin was within 52.6 ng～447.1 ng, r=0.9999 and the sample recovery was 100.06 % (RSD=1.06% (n=9)). CONCLUSION: This method has good repeatability and flexibility. It can be used for quality control of Gegen Qinlian Micropill.
ABSTRACT
AIM: To establish a HPLC method for determination of puerarin and paeoniflorin in Jingfukang Granules(Radix Puerariae, Radix Paeoniae Alba, etc.). METHODS: A Kromasil C 18 Column was used. The mobile phase was methanol water. Puerarin and paeoniflorin were determined by HPLC(dual wavelength, ? 1=250nm,? 2=230nm). RESULTS: The linear range of puerarin was within 99.6ng～996.0ng, r =0.9998, sample recovery was 100.69%, RSD =1.04%( n =9), respectively. The linear range of paeoniflorin was within 119.6ng～ 1315.6 ng, r =0.9999, sample recovery was 100.30%, RSD =1.24%( n =9), respectively. CONCLUSION: This method is simple, reliable and has good repeatability. It can be used for quality control of Jingfukang Granules in production.