A non-aqueous reversed phase HPLC was developed for determining alpha-tocopherol in Sea buckthorn oil capsule without the need for saponification. A reversed phase column (Alltima C(18), 4.6 x 250 mm, 5 microm) was used with a mobile phase of methanol-acetonitrile (95 : 5, v/v) and flow rate of 1 ml/min. The contents in capsule were extracted with n-hexane. Detection wavelength was set at 292 nm. Each analysis requires no longer than 20 min. The linearity range for alpha-tocopherol was 9.4-47.0 microg/ml. The detection limit was 0.94 microg/ml. The mean recovery was 95.82 (RSD 2.3%). This method is suitable for quantitative analysis of alpha-tocopherol in Sea buckthorn oil or its Traditional Chinese Medicinal preparation. 相似文献
A sensitive and specific liquid chromatography–electrospray ionization–tandem mass spectrometry method has been developed and validated for the quantification of huperzine A in human plasma. After the addition of trimetazidine, the internal standard (IS) and sodium hydroxide, plasma samples were extracted using 5 mL ethyl acetate. The compounds were separated on an Agilent Zorbax SB C18 column (100 mm × 2.1 mm ID, dp 3.5 μm) using an elution system of 10 mM ammonium acetate solution–methanol–formic acid (18:82:0.1, v/v) as the mobile phase. The quantification of target compounds was obtained by using multiple reaction monitoring (MRM) transitions: m/z 243.1, 210.1 and 267.2, 166.0 were measured in positive mode for huperzine A and IS. Linearity was established for the range of concentrations 0.01–4.0 ng mL?1 with a coefficient of correlation (r) of 0.9991. The lower limit of quantification (LLOQ) was identifiable and reproducible at 0.01 ng mL?1. The method has been successfully applied to study the pharmacokinetics of huperzine A in healthy male Chinese volunteers. 相似文献
The qualitative and quantitative capability of the ion trap mass analyzer could be greatly affected by the accumulation time. However, the importance of the accumulation time has not so far been thoroughly explored. Here, the influence of ion accumulation time on qualitative and quantitative analysis of complicated components was systematically investigated based on the case study of 40 ophiopogonins in Ophiopogon extract by hybrid ion trap time-of-flight mass spectrometry (LCMS-IT-TOF). In this process, the accumulation time was set at 10, 25, 50, 100, and 200 ms, respectively. The effect of accumulation time on qualitative analysis of ophiopogonins was studied by comparing the total ion current (TIC) of MS1, TIC of MS2, and the number and signal of fragmental ions. The results demonstrated that the signal could be greatly influenced by varying the accumulation time. The number and signal of the fragmental ions were increased significantly with a longer accumulation time in the range of 10–100 ms. Also, the effect of accumulation time on quantitative analysis of ophiopogonins was investigated by comparing the linearity, accuracy, and precision measured on LCMS-IT-TOF. Importantly, quantitative parameters could all be significantly improved by choosing an appropriate accumulation time.
SHR110008 is a representative 9-β-dihydro-9,10-O-acetal taxane with greater anticancer activity and less toxicity than docetaxel. To support a preclinical study of its pharmacokinetics and to predict the effect of 9-β-dihydro-9,10-O-acetal modification on its pharmacokinetic properties, we have developed a sensitive and rapid liquid chromatographic–tandem mass spectrometric method for quantitative analysis of SHR110008 in rat and dog plasma. Plasma was extracted with ethyl acetate. The analytes were separated on a 150 × 4.6 mm i.d., 5 μm particle, reversed-phase C18 column with 90:10 (v/v) methanol–0.1% formic acid as mobile phase at a flow rate of 0.3 mL min−1. Detection was performed by triple-quadrupole tandem mass spectrometry in selected reaction monitoring (SRM) mode with an electrospray ionization source. The precursor-to-product ion transition m/z 933 → 142 was used. The method was validated for accuracy and precision, and linearity in the two matrices was good. Lower limits of quantification (LLOQ) in rat and dog plasma were 5 and 2 ng mL−1, respectively. There were no stability-related problems in the procedure for analysis of SHR110008. The method was successfully used in a preclinical study of the pharmacokinetics of SHR110008 in rats and beagle dogs. The pharmacokinetics of SHR110008 were non-linear in rats and dogs. The elimination half-life ranged from 5.18 to 7.32 h for the rats and from 6.42 to 8.42 h for the dogs.
This paper reports a sensitive, specific, and stable chromatographic procedure with selective detection (electrospray mass
spectrometry in selected-ion-monitoring mode) combined with simple and efficient sample preparation for determination of icariin
in rat plasma after administration of Herba Epimedii. Separation of the analyte, possible endogenous compounds, and constituents
of Herba Epimedii were accomplished on a 250 mm × 2.0 mm i.d. C18 column by use of a rapid gradient. Ionization of icariin and clarithromycin (internal standard) was achieved by use of the
electrospray interface in positive-ion mode. Conditions such as ionization mode, type of organic modifier, eluent additives,
and Q-array potential were optimized to achieve good sensitivity and specificity of icariin detection. Response was a linear
function of concentration over the range 0.2–20 ng mL−1. The method is accurate and precise; within-batch and between-batch precision (CV) are <15%, and accuracy (RE) is better
than ±15%. The method can be used for analysis of icariin in plasma after administration of Herba Epimedii or of traditional
Chinese medicinal preparations containing Herba Epimedii. 相似文献
A simple, rapid and reliable high-performance liquid chromatographic method was developed and validated for the determination of pirfenidone and its major metabolites in rat plasma. Plasma proteins were precipitated with perchloric acid (10%, v/v) and the supernatant after centrifugation was determined using high-performance liquid chromatography. The analysis was carried out on a Lichrospher C(18) column (250 x 4.6 mm i.d., 5 microm). The mobile phase consisted of acetonitrile-water containing 0.2% acetic acid (23:77, v/v) at a flow-rate of 1 mL/min. The eluant was detected at 310 nm. The calibration curves were linear over a concentration range from 0.15 to 76.67 microg/mL. The accuracy (relative error) of the assay ranged from -2.6 to 7.9% and the precision (coefficient of variation) was less than 4.5%. The established method has been successfully applied to a pharmacokinetic study of pirfenidone following a single oral dose to rats. 相似文献
Following the seminal work of Xi on the definition of fuzzy ideal in BCI-algebras, three new kinds of definitions of fuzzy
ideal of BCI-algebras are proposed. First, by the use of the relations between fuzzy points and fuzzy sets, the definition
of a (s,t]-fuzzy ideals of BCI-algebras is introduced. The acceptable nontrivial concepts obtained in this manner are the
- fuzzy ideals and
-fuzzy ideals. Second, based on the concept of falling shadow, a theoretical approach of fuzzy ideal is established and the
fuzzy ideal based on t-norm is proposed. Finally, by the use of the implication operators of fuzzy logic, an R-fuzzy ideals
is proposed and relations between the (s,t]-fuzzy ideals and R-fuzzy ideals are discussed.
*Foundation Item:Supported by NNSF of China(60274016). Biography:Zhang Guang-ji(1947-),male,Professor 相似文献