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Objective:To establish an HPLC-DAD-ELSD method for the simultaneous determination of eight main active components in Buyang Huanwu Decoction, including hydroxysafflor yellow A, paeoniflorin, calycosin glycoside, ferulic acid, ononin, calycosin, fermononetin and astragaloside.Methods:Agilent Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) was used with acetonitrile-0.1% formic acid as the mobile phase. The flow rate was 1.0 ml/min; the column temperature was 30 ℃; the detection wavelengths were 230 nm (paeoniflorin), 254 nm (calycosin glycoside, ononin, calycosin, fermononetin), 322 nm (ferulic acid) and 403 nm (hydroxysafflor yellow A); the drift tube temperature of the evaporative light scattering detector was 60 ℃; the carrier gas flow rate was 1.6 L/min.Results:Under these conditions, the separation of hydroxysafflor yellow A, paeoniflorin, calycosin glycoside, ferulic acid, ononin, calycosin, fermononetin and astragaloside was good, and the linear relationship was in line with the requirements ( r=0.994 0-0.999 9). The average recovery was 97.8% - 101.4% ( RSD was 1.28% - 3.70%). Conclusion:The method is simple, stable and reproducible, and can be used for the quality control of Buyang Huanwu Decoction.
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To improve the quality control methods of Poria and develop and utilize its resources fully, alkaline extraction was used in this study to determine the yield and content of alkali-soluble polysaccharides of Poria. The alkali-soluble extracts of Poria were obtained according to the optimum extraction conditions on the basis of single-factor test, and 30 batches of samples were determined. The structure and chemical composition of the alkali-soluble extracts was characterized by high-performance gel permeation chromatography(HPGPC), Fourier transform infrared spectrometry(FT-IR), nuclear magnetic resonance(NMR) spectroscopy and high-performance liquid chromatography(HPLC) with 1-phenyl-3-methyl-5-pyrazolone(PMP-HPLC). The results showed that the content of the alkali-soluble extracts was in the range of 46.98%-73.86%. The main component was β-(1→3)-glucan, and its molecular mass was about 1.093×10~5. Further, the content of alkali-soluble polysaccharides of Poria was measured by UV-Vis spectrophotometry and HPLC coupled with the evaporative light scattering detector(HPLC-ELSD), and 30 batches of samples were measured. The results indicated that the content of alkali-soluble polysaccharides determined by UV-Vis spectrophotometry was in the range of 73.70%-92.57%, and the content of samples from Hubei province was slightly higher than that from Yunnan province, Anhui province and Hunan province. The content of alkali-soluble polysaccharides determined by HPLC-ELSD was in the range of 51.42%-76.69%, and the samples from Hunan province had slightly higher content than that from the other three provinces. The content determined by UV-Vis spectrophotometry was higher than that by HPLC-ELSD. However, the content determined by HPLC-ELSD was close to that of alkali-soluble extract, which could accurately characterize the content of alkali-soluble polysaccharides in Poria, and the method was simple and repeatable. Therefore, it is recommended that the quantitative analysis method for alkali-soluble extract and alkali-soluble polysaccharides by HPLC-ELSD be used in the quality standards of Poria in Chinese Pharmacopeia.
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Poria/chemistry , Spectroscopy, Fourier Transform Infrared , China , Polysaccharides/chemistry , Reference Standards , Chromatography, High Pressure Liquid/methodsABSTRACT
ObjectiveTo study the effect of flower removal on the content of three alkaloids in different parts of Fritillaria thunbergii from different regions and at different growth stages. MethodThe content of peiminine， peimine， and peimisine in the bulb， root， stem， and leaf of F. thunbergii after flower removal and with flower un-removed at different growth stages and in different regions were determined simultaneously by ultra-performance liquid chromatography-evaporative light scattering detection （UPLC-ELSD） method. The UPLC was conducted on ACQUITY UPLC BEH C18 column （2.1 mm × 150 mm， 1.7 μm） with the mobile phase of 0.02% triethylamine aqueous solution （A） and methanol （B）elution gradient（0-2 min， 45%A； 2-5 min， 45%-25%A； 5-7 min， 25%A； 7-17 min， 25%-10%A； 17-20 min， 10%A）， flow velocity of 0.20 mL·min-1， column temperature 35 °C， sample room temperature of 20 °C， and injection volume of 3 µL. The ELSD was carried out at drift tube temperature 45 °C and with the sprayer parameter of 40%. ResultThe flower removal significantly increased the yield of F. thunbergii. At the budding stage， the alkaloid content in the bulb of F. thunbergii from Ningbo in Zhejiang， Pan'an in Zhejiang， and Nantong in Jiangsu after flower removal were significantly higher than that of flowering un-removal treatment， while it showed no significant difference between the flower removal and un-removal treatments for the samples from Fengjie in Chongqing. At the flowering stage， the alkaloid content in the bulb of F. thunbergii from Nantong in Jiangsu after flower removal was significantly higher than that of flower un-removal treatment， while it showed an opposite trend for the samples from Pan'an in Zhejiang and Fengjie in Chongqing and had no significant difference between the two treatments for the samples from Ningbo in Zhejiang. At the bulb expansion stage， the alkaloid content in the bulb of F. thunbergii from Ningbo in Zhejiang and Pan’an in Zhejiang after flower removal were significantly higher than that of flower un-removal treatment， which was opposite for the samples from Nantong in Jiangsu and had no significant difference between the treatments for the samples from Fengjie in Chongqing. At the harvest stage， except for the samples from Pan'an in Zhejiang， the samples from the rest 3 regions showed decreased alkaloid content in the bulb after flower removal compared with that of flower un-removal treatment. The alkaloid content in the leaf was higher than that in the bulb of F. thunbergii at all growth stages and from different origins. ConclusionFlower removal can increase the yield of F. thunbergii. The alkaloid content in the bulb of F. thunbergii with flower removed was higher than that with flower un-removed at the budding stage， while this trend was reversed at the harvest stage. Both the yield and the alkaloid content of F. thunbergii from Pan'an in Zhejiang were increased by flower removal. The above-ground part of F. thunbergii has a potential development value.
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Photothermal therapy has the characteristics of minimal invasiveness, controllability, high efficiency, and strong specificity, which can effectively make up for the toxic side effects and tumor resistance caused by traditional drug treatment. However, due to the limited tissue penetration of infrared light, it is difficult to promote and apply in clinical practice. The eye is the only transparent tissue in human, and infrared light can easily penetrate the eye tissue, so it is expected that photothermal therapy can be used to treat fundus diseases. Here in, a new nano-platform assembled by liposome and indocyanine green (ICG) was used to treat retinoblastoma. ICG was assembled in liposomes to overcome some problems of ICG itself. For example, ICG is easily quenched, self-aggregating and instability. Moreover, liposomes can prevent free ICG from being cleared through the systemic circulation. The construction of the nano-platform not only ensured the stability of ICG in vivo, but also realized imaging-guide photothermal therapy, which created a new strategy for the treatment of retinoblastoma.
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Objective To establish a method for the simultaneous determination of new mangiferin, mangiferin, artemisinin BⅡ, icariin and artemisinin A in Anemarrhenae Rhizoma by high performance liquid chromatography-evaporation light scattering detector (HPLC-ELSD). Methods The column was Agilent Poroshell 120 EC-C18. The mobile phase used acetonitrile-0.2% acetic acid water system with gradient elution. Column temperature was 30 ℃. Flow rate was 0.7 ml/min. Evaporative light scattering detector used nitrogen as atomizing gas. The atomizing gas temperature was 40 ℃ and the drift tube temperature was 90 ℃. The nitrogen volume flow rate was 2.00 L/min and the sample volume was 20 μl. Results The five components were able to achieve baseline separation. Neomangiferin, Mangiferin, Anemaponin BⅡ, Baohuoside I , Anemarrhena saponin AⅢwere determined as 24.1-386 μg/ml (r=0.999 3), 23.2-371 μg/ml (r=0.998 6), 54.2-867.2 μg/ml(r=0.995 6), 5.3-84.8 μg/ml (r=0.996 8), 10-160 μg/ml (r=0.998 9) respectively, which showed a good linear relationship within the concentration range. The average recovery rate of the five components was between 101.8% and 105.0%, and the repeatability RSD was less than 2.4%. The content of the above five components in Zhimu medicinal materials were 1.62%, 0.82%, 7.36%, 0.07%, 0.34%, respectively. Conclusion The method is simple, accurate, and highly sensitive, which could be used as the quantitative determination of multiple index components of Anemarrhenae Rhizoma.
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Objective:To investigate the factors that could influence the particle size and size distribution of mRNA vaccines.Methods:The influences of several factors including the ionic strength and pH values of buffers, solutions, dilution folds and testing equipments on the particle size and size distribution of three batches of mRNA vaccines were analyzed by dynamic light scattering.Results:The particle size increased with increasing ionic strength, but no significant change in size distribution was observed. The particle size also increased with increasing pH values and the size distribution showed significant change when the buffer solution was weakly alkaline. Solution types could affect the particle size, but had no influence on size distribution. There was no significant change in the particle size or size distribution when the dilution was limited to 100 folds. Moreover, the particle size and size distribution detected by different equipments showed no significance difference.Conclusions:The particle size and size distribution of mRNA vaccines could be affected by solution, dilution fold and testing equipment, which should be concerned during the vaccine production and quality control.
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Objective:To evaluate the ability of light dispersive colorimetry to detect hemoglobin (Hb) in lipid blood samples and its feasibility as an alternative to plasmapheresis commonly used in the laboratory.Methods:Routine blood samples of 276 inpatients in Fujian Provincial Hospital from July 2020 to July 2021 were collected. Routine blood samples of 276 inpatients were collected. There were 169 males and 107 females, aged from 16 to 97 years. 183 non-lipid blood samples and 93 lipid blood samples were collected.(1) One case each of low, medium and high Hb value in non-lipid blood and lipid blood samples were collected, and the precision and the linearity of light scattering method was detected.(2)Non-lipid blood samples divided into Hb low-value group, median-value group and high-value group, which were measured by light scattering method and colorimetric method to compare Hb values. (3)Non-lipid blood samples were divided into Hb low-value group, median-value group and high-value group. Plasma exchange was carried out with different concentrations of fat emulsion. The bias and linearity of Hbc2 and Hbc1, Hbo2 and Hbc1 were analyzed by MedCalc19.1 software. The Hbc2 and Hbc1 bias ( CV%) and Hbo2 and Hbc1 bias ( CV%) were calculated. T test was used to analyze the influence of different concentrations of triglyceride on Hb bias.(4)Blood samples were divided into Hb low-value group, median-group and high-value group. The Hb of light scattering method was compared with the colorimetric method after plasma exchange. Results:(1)The intrabatch precision of light scattering method for non-lipid blood and lipid blood specimens was within the allowable range ( CV<1.5%), and the good linearity ( R2=1.000).(2)The bias of Hb measured by light scattering method and colorimetric method in the three groups was below 3.5%(-0.58±2.34,0.16±1.52,1.15±1.56), within the allowable total error range. The two methods have the equivalence and good linear relationship ( r=0.999).(3)The concentrations of Hbo2 in the low (except 4.1 mmol/L), medium and high Hbo2 groups were equivalent to those in the non-lipid blood colorimetry (Hbc1), and the two methods were well correlated. The results of light scattering method have nothing to do with the concentration of lipid blood.(4)There was no significant difference of the Hb between the light scattering method and plasma exchange method in three groups ( P>0.05), Both of them have equivalence and good correlation ( R2=0.968,0.948,0.870). Conclusion:Light scattering method can effectively reduce the effect of lipid blood on hemoglobin determination, and can replace the traditional plasma exchange method, which has high clinical application value.
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The aim of this study is to develop the first simultaneous method for quantification of neomycin and polymyxin B inthe presence of dexamethasone using High Performance Liquid Chromatography (HPLC) with an Evaporative LightScattering Detector (ELSD). The analysis was performed using a phenyl Waters X Bridge column, an evaporationtemperature of 50oC, and a nitrogen pressure of 320 kPa. The mobile phase consists of a combination of methanoland trichloroacetate acid (40 mM, pH 1.70–1.80) in gradient mode, flow rate at 1.0 ml/minute, detector gain of 6,and analysis time of 35 minutes. The linearity was achieved with a concentration of 100–500 µg/ml (r = 0.99955)for neomycin and concentration of 30–100 µg/ml (r = 0.99703) for polymyxin B. Recovery results were obtainedbetween 99.150% and 104.773% for neomycin and 96.538% and 105.139% for polymyxin B. The analysis samplefrom the market was found to be 102.27% for neomycin and 100.79% for polymyxin B. The result was compared tothe standard microbiological method. Based on the T-test results of two samples with a 95% confidence level (α =0.05), it was concluded that there was no significant difference between HPLC-ELSD and microbiological methodsfor determining neomycin and polymyxin B. The HPLC-ELSD method has a potential for routine analysis due toadvantages in terms of increasing precision, accuracy, and shorter testing time.
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The resonance light scattering (RLS) spectral characteristics of the interaction between rose Bengal and mexiletine hydrochloride in the presence of cetylpyridinium bromide were investigated. A dual-wavelength resonance light scattering (DWO-RLS) method for the determination of mexiletine hydrochloride in drugs was established. In a weakly acidic solution, rose Bengal interacts with mexiletine hydrochloride and cetylpyridinium bromide to form a red ternary ion association complex, which led to a significantly enhanced resonance light scattering signal and produced two strong characteristic scattering peaks at 372 nm and 596 nm. In these two wavelengths the mass concentration of mexiletine hydrochloride was in the range of 0.004 to 0.65 mg·L-1 and had a good linear relationship with the resonance light scattering enhancement intensity (ΔIRLS), with detection limits of 0.003 2 mg·L-1 (372 nm) and 0.003 8 mg·L-1 (596 nm), respectively. When measured by the dual-wavelength resonance light scattering (DWO-RLS) technique, the detection limit was lower, only 0.001 8 mg·L-1. When the DWO-RLS method was applied to the determination of mexiletine hydrochloride in commercially available mexiletine hydrochloride tablets, and the recovery was 98.5%-103%, and the relative standard deviation was 2.0%-2.7%.
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italic>K-values of 56 batches of 7 types of povidone were measured by microfluidic rheometry and with a Ubbelohde capillary viscometer. The K-values of the two methods were tested by SPSS software and the results showed that there was no significant difference between the two methods (P > 0.05). Taking K-values measured with the Ubbelohde capillary viscometer (Ku) as the abscissa and K-values measured by microfluidic rheometry (Km) as the ordinate a linear equation was calculated: Km = 0.893 9Ku + 4.617 6, R2 = 0.986 2, with good linearity, indicating that the microfluidic rheometer method can replace the Ubbelohde capillary viscometer in determining K-values of povidone. The microfluidic rheometer method has the benefits of less sample consumption, faster determination, and is more accurate, and it can be used with high-throughput automatic acquisition, which provides a more convenient method for the determination of K-values of different types of povidone. The weight-average molecular weights (Mw) of each type of povidone were measured by gel permeation chromatography-multi angle laser light scattering (GPC-MALLS), and the relationship between Mw and Km was lgMw = -0.000 4 Km2 + 0.072 7 Km + 2.791, R2 = 0.990 1. The fitting relationship was good, and Mw could be calculated by Km by the equation.
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This study aimed to explore the link between block copolymers' interfacial properties and nanoscale carrier formation and found out the influence of length ratio on these characters to optimize drug delivery system. A library of diblock copolymers of PEG-PCL and triblock copolymers with additional PEI (PEG-PCL-PEI) were synthesized. Subsequently, a systematic isothermal investigation was performed to explore molecular arrangements of copolymers at air/water interface. Then, structural properties and drug encapsulation in self-assembly were investigated with DLS, SLS and TEM. We found the additional hydrogen bond in the PEG-PCL-PEI contributes to film stability upon the hydrophobic interaction compared with PEG-PCL. PEG-PCL-PEI assemble into smaller micelle-like (such as PEG-PCL4006-PEI) or particle-like structure (such as PEG-PCL8636-PEI) determined by their hydrophilic and hydrophobic block ratio. The distinct structural architectures of copolymer are consistent between interface and self-assembly. Despite the disparity of constituent ratio, we discovered the arrangement of both chains guarantees balanced hydrophilic-hydrophobic ratio in self-assembly to form stable construction. Meanwhile, the structural differences were found to have significant influence on model drugs incorporation including docetaxel and siRNA. Taken together, these findings indicate the correlation between molecular arrangement and self-assembly and inspire us to tune block compositions to achieve desired nanostructure and drug loading.
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Objective:To establish the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction. Method:Ten batches of Asparagi Radix standard decoction were prepared. High performance liquid chromatography-evaporative light scattering detection method (HPLC-ELSD) was established for the determination of protodioscin and protoneodioscin in Asparagi Radix decoction pieces and its standard decoction, and the fingerprint detection of Asparagi Radix decoction pieces with acetonitrile-water as mobile phase for gradient elution. UHPLC-LTQ-Orbitrap-MS/MS was used to identify ten main common peaks in the fingerprint with acetonitrile-0.1% formic acid solution as mobile phase for gradient elution, electrospray ionization (ESI) and positive and negative ion mode scanning were employed, the detection range was m/z 100-1 400. Result:The total content of protodioscin and protoneodioscin in Asparagi Radix decoction pieces was 0.41%-0.72%, and their total content in Asparagi Radix standard decoction was 0.33%-0.59%, the transfer rate of these two components was 73.6%-98.3%. The dry extract yield of the standard decoction was 59.0%-73.0%, and its pH was 4.9-5.6. There were 10 common peaks in the fingerprint, and all of them were saponins, including protoneodioscin, protodioscin, aspacochioside A and its isomer, methyl protodioscin, asparagoside F, (25R)-26-O-β-D-glucopyranosyl-furostan-5, 20-diene-3β, 26-diol-3-O-[α-L-rhamnopyranosyl (1→2)]-[β-D-glucopyranosyl (1→4)-α-L-rhamnopyranosyl (1→4)]-β-D-glucopyranoside, 26-O-β-D-glucopyranosyl-furostan-20 (22)-ene-3β, 26-diol-3-O-[α-L-rhamnopyranosyl (1→2)]-[α-L-rhamnopyranosyl (1→4)]-β-D-glucopyranoside, pseudodiosgenin, aspacochioside C. Conclusion:In this paper, the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction are established, and these methods are stable and feasible, which can provide reference for the quality control of pharmaceutical preparations containing Asparagi Radix.
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BACKGROUND: Whole-body cell analysis of organisms is one of the major challenges in biomedicine. Tissue optical clearing technique combined with optical imaging and image processing technique can make the whole organ or the body transparent rapidly for structural and cellular analyses, providing a very promising solution for the application of advanced optical technique in life science. OBJECTIVE: To analyze the principle and process of tissue optical clearing technique, to summarize the research progress of tissue optical clearing technique, to present imaging technology for tissue clearing, and to discuss the application of tissue optical clearing technique in biomedical researches. METHODS: The first author searched relevant literatures in PubMed database with the keywords of “tissue optical clearing technique, tissue optical clearing, whole-body imaging and 3D imaging”. A total of 168 articles were initially retrieved. After sorting and screening systematically, 72 literatures were included for analysis, summary and discussion. RESULTS AND CONCLUSION: Current tissue optical clearing protocols are divided into two groups: solvent-based clearing methods and hydrophilic reagent-based clearing methods. Tissue clearing is usually conducted by the following steps: (a) tissue fixation, (b) permeabilization, (c) decolorization, and (d) refractive index matching. Tissue optical clearing technique can rapidly transform tissue into an optically transparent form, improving imaging depth and contrast. Combined with microscope imaging techniques such as confocal, two-photon and light sheet microscopes, tissue clearing can achieve 3D imaging of the whole organ or body at cellular resolution, accelerating the process of whole-body cell analysis of organisms. Tissue optical clearing technique will continue to evolve in the future, promote the development of new clearing reagents and clearing optimized microscopes, further enhance the acquisition of structural and molecular information from intact systems and contribute to the comprehensive understanding of whole biological systems.
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Evaporative light scattering detector(ELSD) and charged aerosol detector(CAD) methods were established in this study for the content determination of four kinds of sugars in Zhusheyong Yiqi Fumai(YQFM), and the factors affecting the accuracy of CAD methods were discussed. HPLC-ELSD chromatographic separation was performed on a Shodex Asahipak NH2 P-50 column with acetonitrile-water(75∶25)as the mobile phase, with a flow rate of 0.8 mL·min~(-1), drift tube temperature of 80 ℃. The analysis by HPLC-CAD was performed on the same column with acetonitrile-water as mobile phase for gradient elution, with a flow rate of 0.8 mL·min~(-1), a neb temperature of 45 ℃, and power function(PF) of 1.3. The samples of YQFM were detected by ELSD and CAD respectively. It was found that YQFM was composed of fructose, glucose, sucrose and maltose. The linear relationship of the two methods was good, and the recoveries, reproducibility and stability of these four kinds of sugars measured by the two methods satisfied the requirements of methodology. Both CAD and ELSD detectors were accurate and reliable in detecting saccharides components in YQFM. In addition, it was revealed in this study for the first time that the PF parameter of CAD had an important influence on the accuracy of sugar determination and acted as the key parameter of CAD method. It was also found that for CAD, a non-linear detector, there was no significant difference between the results of linear regression and logarithmic regression.
Subject(s)
Aerosols , Carbohydrates , Chromatography, High Pressure Liquid , Light , Reproducibility of Results , Scattering, Radiation , SugarsABSTRACT
To determine relative molecular weight of astragalus polysaccharides (APs), we used Shodex GS620 gel permeation chromatographic column and differential refraction detector (GPC-RI) with dextran as a reference. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and GPC combined with multi-angle laser light scattering detection (GPC-MALLS) were also used．GPC-RI measure showed four peaks of APs, with the Mw of 1 380 000, 231 000, 18 000, and 480, respectively. Three main peaks were found by GPC-RI-MALLS with the Mw as 1 148 000, 180 000, and 43 000, respectively. Strong signals in 155 000 and 18 000 were detected by MALDI-TOF-MS, which also indicated the sugar moieties of the APs as hexoses. From our study, we found that the GPC-RI method with universal correction is most suitable for Mw determination of the APs. Nevertheless, the three methods should be combined and contrasted with each other to obtain accurate information in research of polysaccharides from Chinese medicine.
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Objective: To establish a simple,rapid and novel Rayleigh light scattering(RLS)method for rapid determination of mexiletine hydrochloride in drugs. Methods: In the presence of acid Tris-HCl medium and cetylpyri- dinium bromide,eosin Y reacted with mexiletine hydrochloride to form a ternary ion association complex with two charac- teristic scattering peaks by electrostatic attraction. The detection wavelengths were 368 and 586 nm. There was a linear relationship between the mexiletine hydrochloride concentration in a certain range and the Rayleigh light scattering en- hancement intensity(ΔIRLS)of the association complex. Single-wavelength Rayleigh scattering(SWO-RLS)method or dualwavelength Rayleigh light scattering(DWO-RLS)method was used to determine the content of mexiletine hydrochloride, and the mexiletine hydrochloride content was calculated according to the regression equation of standard curve. Results: The linear ranges of mexiletine hydrochloride were 0.005-0.65 mg/L(SWO-RLS method,368 nm),0.004-0.65 mg/L (SWO-RLS method,586 nm)and 0.004-0.65 mg/L(DWO-RLS method,368 nm+586 nm),respectisely. Detection lim- its were 0.0033(SWO-RLS method,368 nm),0.0040(SWO-RLS method,586 nm)and 0.0018 mg/L(DWO-RLS method, 368 nm+586 nm),respectisely. The recovery and relative standard deviation(RSD,n=5)for a SWO-RLS method were 98.6-103% and 1.4-1.8%,respectively(SWO-RLS method,368 nm). Conclusion: The method is simple,rapid, highly sensitive and high selectie.
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Background: A simple and efficient strategy for agarase immobilization was developed with carboxyl-functionalized magnetic nanoparticles (CMNPs) as support. The CMNPs and immobilized agarase (agarase-CMNPs) were characterized by transmission electron microscopy, dynamic light scattering, vibrating sample magnetometry, scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, and zeta-potential analysis. The hydrolyzed products were separated and detected by ESI-TOF-MS. Results: The agarase-CMNPs exhibited a regular spherical shape with a mean diameter of 12 nm, whereas their average size in the aqueous solution was 43.7 nm as measured by dynamic light scattering. These results indicated that agarase-CMNPs had water swelling properties. Saturation magnetizations were 44 and 29 emu/g for the carriers and agarase-CMNPs, respectively. Thus, the particles had superparamagnetic characteristics, and agarase was successfully immobilized onto the supports. Agaro-oligosaccharides were prepared with agar as substrate using agarase-CMNPs as biocatalyst. The catalytic activity of agarase-CMNPs was unchanged after six reuses. The ESI-TOF mass spectrogram showed that the major products hydrolyzed by agarase-CMNPs after six recycle uses were neoagarotetraose, neoagarohexaose, and neoagarooctaose. Meanwhile, the end-products after 90 min of enzymatic treatment by agarase-CMNPs were neoagarobiose and neoagarotetraose. Conclusions: The enhanced agarase properties upon immobilization suggested that CMNPs can be effective carriers for agarase immobilization. Agarase-CMNPs can be remarkably used in developing systems for repeated batch production of agar-derived oligosaccharides.
Subject(s)
Oligosaccharides/metabolism , Enzymes, Immobilized , Magnetite Nanoparticles/chemistry , Glycoside Hydrolases/metabolism , Thermogravimetry , X-Ray Diffraction , Enzyme Stability , Catalysis , Microscopy, Electron, Transmission , Magnetometry , Dynamic Light Scattering , Glycoside Hydrolases/chemistryABSTRACT
Objective:To establish a laser light scattering method for the determination of the particle size distribution of clostridium butyricum enterococcus triple viable powder and compare the results of the sieving method.Methods:The conditions of laser scattering method were as follows:the vibration sampling rate of 80%,the dispersion pressure of 0.05 MPa,the background and sample scan time of 15 s,the shading of 0.5%-5%,the refractive index of the particles of 1.55,the particle absorption rate of 0.01,and the injection volume of 0.1-0.2 g.The eigenvalues of the particle size distribution were determined,which were the particle size cumulative distribution map of 10%,50% and 90% of the particle size value and the volume average particle diameter D.Results:The RSDs of d(0.1),d(0.5) and d(0.9) were less than 5% in the methodology study.The results of laser light scattering method showed that the particle size of 93.3% samples was below 250 μm,that of 64.2% samples was below 150 μm,that of 51.4% samples was below 125 μm,and that of 31.3% samples was below 90 μm.The results of sieving method showed that the particle size of 96.6% was below 250 μm,that of 46.4% samples was below 150 μm,that of 23.5% samples was below 125 μm,and that of 1.4% samples was below 90 μm.Conclusion:Sieving method and laser light scattering method both can characterize the particle size distribution of the sample.The laser light scattering method is simple,accurate and producible,which is suitable for the particle size control of clostridium butyricum enterococcus triple viable powder.
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OBJECTIVE:To establish the method for the determination of particle size distribution of Budesonide nasal spray, and to analyze the consistency of particle size distribution of spray samples. METHODS:Water was used as dispersant for mixing and dispersing(1800 r/min). The particle sizes [d(0.1),d(0.5),d(0.9)] corresponded to accumulative particle size of 10%,50%and 90%were used as characteristic value. The distribution of granularity was determined by laser scattering method. The consisten-cy of particle size distribution of samples from 2 manufacturers (A,B) were analyzed among different batches or same batch of same manufacturer by SAS 9.3 statistical software. RESULTS:The mean values of d(0.1),d(0.5) and d(0.9) were 3.96 μm, 29.58 μm and 67.10 μm in manufacturer A. The mean values of d(0.1),d(0.5)and d(0.9)were 2.00 μm,7.53 μm and 28.51 μm in manufacturer B. By analysis,there was great difference in particle size of samples from 2 manufacturers. The particle size of the samples from manufacturer A were larger than that of manufacturer B. The consistency among different batches from manufacturer B was better,and the consistency among same batch were all good from 2 manufacturers. CONCLUSIONS:The established meth-od is suitable for particle size distribution of Budesonide nasal spray and the consistency analysis of particle size distribution.
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Objective To establish the quality standard ofQizhu-Fuzheng Yin, and to conduct a preliminary study on its stability.Methods Corydalis tuber and licorice were identified by TLC. The content of astragaloside was determined by UPLC-ELSD. The initial stability was studied by accelerated test method. Results The spots on TLC plates were clear without interference in the blank reference. The response of astragaloside was linear in the ranges of 36.5-365.0 μg/ml (r2=0.999 2), and the average recovery was 102.8 %, and theRSD was 2.4%. After 1, 2, 3, 6 months tests, the average contents of 3 batches astragaloside were 61.6, 60.4, 60.6μg/ml.ConclusionQizhu-Fuzheng Yin was simple preparation, quality control and stability.