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- Author or Editor: W. Liu x
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Shenqi Fuzheng Injection (SFI) is a traditional Chinese medicine injection, widely used to enhance immune function of clinical cancer patients undergoing chemotherapy. In this study, a high-performance liquid chromatography-diode array detection-evaporative light scattering detection (HPLC-DAD-ELSD) method was established for quality control of SFI, which could simultaneously semiquantitatively reflect the constituents displayed in the chromatographic profile of SFI. The relative retention time and relative peak areas of the 21 common peaks related to the reference peak were calculated. The validity and advantage of this method were validated by systematically comparing chromatograms of 10 batches of SFI samples with the analytical methods of principal component analysis and angle cosine method recommended by the State Food and Drug Administration of China. Moreover, a total of 21 constituents of SFI were identified or tentatively characterized in the fingerprint via ultrafast liquid chromatography-diode array detection-quadrupole time-of-flight (UFLC-DAD-Q-TOF) tandem mass spectrometry technique on the basis of the retention time, ultraviolet spectra, fragmentation patterns, and reported literatures. All the results proved that the technique was useful in comprehensive quality evaluation of SFI and further study.
Summary
Oroxylin A (5,7-dihydroxy-6-methoxyflavone), which has showed multiple pharmacological effects, was semi-synthesized chemically as a pharmaceutical agent. Its impurities, degradation products and their formation pathways remain unknown. In the present study, two impurities (5,6,7-trihydroxyflavone, 5-hydroxy-6,7-dimethoxytlavone) and a degradation product (5,7-dihydroxy-8-methoxyflavone) in Oroxylin A bulk drug substance were identified, and their formation pathways were proposed. A reversed phase liquid chromatographic method for the simultaneous determination of Oroxylin A and the three compounds was developed on a C18 column using methanol-acetonitrile-0.1% acetic acid (54:23:23, v/v/v) as the mobile phase. The detection was performed at 271 nm. The method was validated to be robust, precise, specific and linear between 4 and 40 μg mL−1; the limits of detection and quantification of Oroxylin A were 0.01 and 0.04 μg mL−1, respectively. The developed method was found to be suitable to check the quality of bulk samples of Oroxylin A at the time of batch release and also during its stability studies (long term and accelerated stability).
Summary
10-O-(N,N-dimethylaminoethyl)-ginkgolide B (XQ-1) is an intermediate for synthesizing 10-O-(N,N-dimethylaminoethyl)-ginkgolide B methanesulfonate (XQ-1H), which is a novel ginkgolide B derivative and is being developed as a platelet-activating factor antagonist. A specific and rapid liquid chromatographic method was developed for the quantitative analysis of XQ-1 and its three related impurities, which were 10-O-(N,N-dimethylaminoethyl)-11,12-seco-ginkgolide B (imp-1), 10-O-(N,N-dimethylaminoethyl)-11,12-seco-3,14-dehydroginkgolide B (imp-2) and 10-O-(N,N-dimethylaminoethyl)-3,14-dehydroginkgolide B (imp-3) simultaneously in XQ-1 samples. Chromatographic separation was achieved on a CN band stationary phase, with the mobile phase consisting of methanol and 20 mM dipotassium hydrogen phosphate (pH 7.5) (50:50, υ/υ) in isocratic elution. The flow rate was 1.0 mL min−1 and detector was set at 220 nm. The method was optimized by the analysis of the samples generated during the forced degradation studies. The XQ-1, imp-1, imp-2, and imp-3 were completely separated within 15 min. The resolutions (R s) amongst four target compounds were >2. The developed method was validated with respect to specificity, linearity, accuracy, precision, and robustness. The results indicated that the simultaneous LC determination method was readily utilized as a quality control method for XQ-1 sample.
Summary
A preparative high-speed countercurrent chromatograph (HSCCC) method for the isolation and purification of C6-C2 natural alcohol and benzyl ethanol from Forsythia suspensa was successfully established. Cornoside, forsythenside F, forsythiaside, and acteoside were rapidly obtained for the first time by HSCCC with a two-phase solvent system ethyl acetate-n-butanol-methanol-water (5:1:0.5:5, υ/υ) in one-step separation. The purities of them were all above 97% as determined by high-performance liquid chromatography, and the combination of ESI-MS and NMR analysis confirmed the chemical structures of the four compounds.
Summary
A simple and rapid HPLC method using a photodiode array (PDA) detector for the analysis of 3-hydroxycarboplatin and its related complex has been established for the first time. Separation of 3-hydroxycarboplatin and 3-hydroxy-1,1-cyclobutanedicarboxylic acid (3-HO-cbdca) was carried out on a Phenomenex ODS3 column using an aqueous solution containing 50 mM ammonium acetate and 5 mM sodium 1-octanesulfonate as the mobile phase. The flow rate was 0.8 mL min−1, the column temperature was 40°C, and the detection wavelength was 230 nm for 3-hydroxycarboplatin and 220 nm for 3-HO-cbdca. Different analytical performance parameters such as precision, accuracy, linearity, stability of the solution, specificity, limit of detection (LOD), limit of quantification (LOQ), and system suitability were determined using the Empower 2 software. The calibration curve of standard 3-hydroxycarboplatin showed good linearity (r = 0.9995) within the range 0.5–1.4 mg mL−1. The method was accurate and precise, with an average accuracy of 100.4% (RSD = 1.53%, n = 9), and the results of the system suitability test showed symmetrical peaks, good resolution (R s), and repeatability. It can be applied to the quality control of 3-hydroxycarboplatin.
Compound danshen preparations (CDPs) are used clinically for the treatment of cardiovascular and cerebrovascular diseases. By using the quantitative analysis of multi-components by single-marker (QAMS) method, sixteen compounds (danshensu, protocatechuic acid, protocatechuicaldehyde, caffeic acid, rosmarinic acid, lithospermic acid, notoginsenoside R1, salvianolic acid B, ginsenoside Rg1, ginsenoside Re, salvianolic acid A, salvianolic acid C, ginsenoside Rb1, ginsenoside Rd, cryptotanshinone, and tanshinone IIA were quantified on an ACQUITY ultraperformance liquid chromatography (UPLC) HSS T3 column (2.1 × 100 mm, 1.8 μm) with the mobile phase consisting of 0.1% formic acid aqueous solution (A) and acetonitrile (B) using a gradient elution at the flow rate of 0.30 mL/min in 30 min at 30°C, which was also validated by UPLC-diode array detection (DAD) and UPLC-electrospray ionization multistage/mass spectrometry (ESI-MS/MS) for assuring the feasibility and accuracy. Tested by robustness experiment under slightly changeable conditions, the stability of relative correction factor (RCF) proved to be stable, with RSDs below 5.69%, except for notoginsenoside R1 with relative standard deviation (RSD) 7.83%. This reliable and convenient QAMS method resolved the problem of standard substance insufficiency and improved the quality assessment of preparations consisting of complex compounds with different chemical structures, such as CDPs.
Abstract
This work used a carrageenan-based thrombosis model to determine the preventative effects of Lactobacillus plantarum YS1 (LPYS1) on thrombus. In thrombotic mice, LPYS1 improved the activated partial thromboplastin time (APTT), while decreasing the thrombin time (TT), prothrombin time (PT), and fibrinogen (FIB) content. In thrombotic mouse serum, LPYS1 decreased the levels of malondialdehyde (MDA), tumour necrosis factor-alpha (TNF-α), interleukin-6 (IL-6), nuclear factor kappa-B (NF-κB), and interleukin-1 beta (IL-1β), while also increasing the activities of superoxide dismutase (SOD) and catalase (CAT). Moreover, LPYS1 upregulated the mRNA expression levels of copper/zinc-SOD (Cu/Zn-SOD), manganese-SOD (Mn-SOD), and CAT in the colon tissues of thrombotic mice, while downregulating those of NF-κB p65, IL-6, TNF-α, and interferon-gamma (IFN-γ) mRNA. In tail vein vascular tissues, LPYS1 suppressed the mRNA expression levels of NF-κB p65, intercellular cell adhesion molecule-1 (ICAM-1), vascular cell adhesion molecule-1 (VCAM-1), and E-selectin. The abundances of both beneficial and pathogenic bacteria were altered by LPYS1. These findings show that LPYS1 has the capacity to protect mice from thrombosis, while also revealing some of the underlying mechanisms of this effect.
Summary
Radix Isatidis has widely useful activities including anti-virus, anti-bacterial. Tryptanthrin, indigo, and indirubin are active ingredients in R. Isatidis. Response surface methodology (RSM)-optimized infrared-assisted extraction (IRAE) was developed and combined with HPLC for simultaneous determination of tryptanthrin, indigo, and indirubin from R. Isatidis. IRAE were investigated through extraction yields of the three components and optimized by RSM. The optimum conditions were as follows: infrared power of 129 W, solid/liquid ratio of 1:40 g/mL, and irradiation time of 22.5 min. IRAE conditions obtained by RSM were not only accurate, but also had practical value reflecting the expected optimization. Subsequently, this novel IRAE method was evaluated by extraction yield of the components of R. Isatidis samples from different regions. Compared with common extraction methods including maceration extraction (ME), reflux extraction (RE), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), IRAE showed higher yield with advantages of no limitation of solvent selection, low cost, convenience under optimum extraction conditions. These results suggested the potential of RSM-optimized IRAE for extraction and analysis of the water-/fat-soluble compositions of Chinese herbal medicine. A simple chromatographic separation for simultaneous determination of tryptanthrin, indigo, and indirubin from Chinese herbal medicine R. Isatidis was performed on a C18 column (Diamonsil 150 mm × 4.6 mm i.d., 5 μm) with a mobile phase isocratic consisting of methanol and water at a flow-rate of 0.8 mL min−1. The retention times of tryptanthrin, indigo, and indirubin were 15.4, 31.9, and 58.6 min, respectively. The linear equations were obtained as follows: y = −3094.5744 + 21208.792x for tryptanthrin (R = 0.9998, 0.9–18.0 μg mL−1), y = 4730.0448 + 30180.567x for indigo (R = 0.9997, 0.5–10.0 μg mL−1) and y = −6582.9045 + 67069.312x for indirubin (R = 0.9997, 0.4–8.0 μg mL−1). The result showed that RSM-optimized IRAE was a simple, efficient pretreatment method for the analysis of complex matrix.
Citri Grandis Exocarpium (CGE) is a traditional Chinese medicine with a variety of biological activities. For efficient quality control of CGE, a simple, rapid, and accurate high-performance liquid chromatographic (HPLC) method was developed for simultaneous determination of four main compounds (naringin, rhoifolin, meranzin hydrate, and isoimperatorin) in this herb. These four compounds were separated on a C18 column by gradient elution with methanol and water. The flow rate was 1.0 mL·min−1, and the detection wavelength was 324 nm. The recoveries of the method ranged from 96.32% to 103.71%, and good linear relationships (r 2 > 0.9998) over relative wide concentration ranges were obtained. Then this validated method was successfully applied to the analysis of nine batches of CGE samples.
Abstract
Nattokinase (NK) is effective in the prevention and treatment of cardiovascular disease. Cucumber is rich in nutrients with low sugar content and is safe for consumption. The aim of this study was to construct a therapeutic cucumber that can express NK, which can prevent and alleviate cardiovascular diseases by consumption. Because the Bitter fruit (Bt) gene contributes to bitter taste but has no obvious effect on the growth and development of cucumber, so the NK-producing cucumber was constructed by replacing the Bt gene with NK by using CRISPR/Cas9. The pZHY988-Cas9-sgRNA and pX6-LHA-U6-NK-T-RHA vectors were constructed and transformed into Agrobacterium tumefaciens EHA105, which was transformed into cucumber by floral dip method. The crude extract of NK-producing cucumber had significant thrombolytic activity in vitro. In addition, treatment with the crude extract significantly delayed thrombus tail appearance, and the thrombin time of mice was much longer than that of normal mice. The degrees of coagulation and blood viscosity as well as hemorheological properties improved significantly after crude extract treatment. These findings show that NK-producing cucumber can effectively alleviate thrombosis and improve blood biochemical parameters, providing a new direction for diet therapy against cardiovascular diseases.
