2.ICP-MS method for the determination of uranium concentration and 235U/238U ratio in urine and its uncertainty evaluation
Liangliang YIN ; Qing TIAN ; Wei HUANG ; Xianzhang SHAO ; Yanqin JI
Chinese Journal of Radiological Medicine and Protection 2017;37(5):376-380
Objective To establish a method of analyzing total uranium and 235U/238U ratio in urine using inductively coupled plasma mass spectrometry (ICP-MS) and uncertainty assessment.Methods Urine sample was digested with HNO3 and H2O2,and total uranium was determined using ICP-MS method directly.The digested urine sample was separated to concentrate uranium with tributyl phosphate (TBP) column,and 235U/238U ratio was analyzed using ICP-MS.The uncertainty was evaluated through sample pre-treatment,measurement and standard curve calculation.Results The recovery of total uranium in urine was 98.4%-102.4%,detection limit was 0.002 μg/L.The relative expanded uncertainty of total uranium concentration in urine was 0.26 (k =2).235 U/238 U ratio was 0.001 1 (k =2).Conclusions This study offers a low detection limit,good recovery and precision method for rapid determination of total uranium and 235U/238 U ratio in urine samples.It is potential used for both in occupational exposure assessment and nuclear emergency situation.The uncertainty evaluation of total uranium and 235U/238U ratio in urine are reliable.
3.Establishment of quality standard for Corni Fructus based on the multiple bioactive constituents.
Sheng GUO ; Jin-ao DUAN ; Shao-qing ZHU ; Da-wei QIAN
China Journal of Chinese Materia Medica 2015;40(15):3017-3021
This study is to establish the methods for determination of iridoid glycosides and triterpenic acids in Corni Fructus and provide technical support for the quality control of Corni Fructus. Morroniside, loganin and sweroside were determined by HPLC-UV method with acetonitrile and 0.1% formic acid as the mobile phase, and the detective wavelength was set at 240 nm. Oleanolic acid and ursolic acid were determined by HPLC-ELSD method with methanol-0.5% ammonium acetate (87:13) as the mobile phase. The results showed that the linear ranges of morroniside, loganin and sweroside were 5.335-213.4 mg · L(-1) (r = 0.9999), 5.515-220.6 mg · L(-1) (r = 1.0000), 1.992-79.68 mg · L(-1) (r = 1.0000), respectively. The average recoveries of the above three iridoid glycosides were 98.49%-99.28% with RSDs of recoveries being less than 2%. The linear ranges of oleanolic acid and ursolic acid were 7.74-154.8 mg · L(-1) (r = 0.9964), 10.82-216.4 mg · L(-1) (r = 0.9996), respectively. The average recoveries of the above two triterpenic acids were 98.11%-99.27% with RSDs of recoveries being less than 3%. The method established in this research is simple, rapid and reliable, and can be used for quality control of Corni Fructus. Furthermore, the research provided experimental data for the improvement of present quality standard of Corni Fructus, which has important significance to guarantee its quality and clinical curative effect.
Cornus
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chemistry
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Drug Stability
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Oleanolic Acid
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analysis
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Quality Control
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Triterpenes
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analysis
4.Identification of phenylpropanoids in ciwujia injection by HPLC-MS.
Jing HUANG ; Qing SHAO ; Yan-Hua XIANG ; Zhi-Wei GE ; Xiao-Hui FAN
China Journal of Chinese Materia Medica 2014;39(13):2513-2520
There are reports about the chemical compounds of Ciwujia herbs, but with no study report about the chemical material basis of Ciwujia injection (CWJI). In this study, LC-MS(n) and LC-Q-TOF-MS techniques were adopted for a qualitative analysis on phenylpropanoids in CWJI. The Ultmate XB-C18 column (4.6 mm x 250 mm, 5 microm) was adopted and eluted with the mobile phase of 0.5% formic acid-water and acetonitrile, with the flow rate at 0.8 mL x min(-1) and the column temperature at 20 degrees C. Based on the data of high-resolution and multi-stage MS, control products and literatures, altogether 54 phenylpropanoids were identified in Ciwujia Injection, including 34 phenylpropanoids, 16 ligans and 4 coumarins. Among them, 28 were reported for the first time in Ciwujia, and 14 compound structures were identified in comparison with the control products. The method established in this study could be used to simply and rapidly identify phenylpropanoids in CWJI. The findings provide scientific data for defining the chemical material basis of CWJI.
Chromatography, High Pressure Liquid
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methods
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Drugs, Chinese Herbal
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chemistry
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isolation & purification
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Eleutherococcus
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chemistry
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Mass Spectrometry
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methods
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Molecular Structure
5.Research about effect of spray drying conditions on hygroscopicity of spray dry powder of gubi compound's water extract and its mechanism.
Jie ZONG ; Qi SHAO ; Hong-Qing ZHANG ; Yong-Lan PAN ; Hua-Xu ZHU ; Li-Wei GUO
China Journal of Chinese Materia Medica 2014;39(4):663-668
OBJECTIVETo investigate moisture content and hygroscopicity of spray dry powder of Gubi compound's water extract obtained at different spray drying conditions and laying a foundation for spray drying process of Chinese herbal compound preparation.
METHODIn the paper, on the basis of single-factor experiments, the author choose inlet temperature, liquid density, feed rate, air flow rate as investigated factors.
RESULTThe experimental absorption rate-time curve and scanning electron microscopy results showed that under different spray drying conditions the spray-dried powders have different morphology and different adsorption process.
CONCLUSIONAt different spray-dried conditions, the morphology and water content of the powder is different, these differences lead to differences in the adsorption process, at the appropriate inlet temperature and feed rate with a higher sample density and lower air flow rate, in the experimental system the optimum conditions is inlet temperature of 150 degrees C, feed density of 1.05 g x mL(-1), feed rate of 20 mL x min(-1) air flow rate of 30 m3 x h(-1).
Desiccation ; methods ; Drugs, Chinese Herbal ; chemistry ; Hydrophobic and Hydrophilic Interactions ; Particle Size ; Powders ; chemistry ; Temperature ; Water ; analysis ; Wettability
6.Determination of uranium in drinking water in the vicinity of nuclear power plants by ICP-MS
Qing TIAN ; Yanqin JI ; Liangliang YIN ; Wei HUANG ; Xianzhang SHAO ; Baoming SHEN ; Xu SU
Chinese Journal of Radiological Medicine and Protection 2011;31(2):160-162
Objective To ascertain the concentrations of uranium in drinking water around nuclear power plants.Methods A total of 106 water samples were collected from June 2009 to March 2010 in Jiangsu,Zhejiang,Liaoning and Shandong provinces.Inductively coupled plasma-msgs spectrometry(ICPMS)was applied to determine uranium content in local water source and drinking water.The detection limit of U was 0.8 ng/L.The recovery was 100.9%.Results The uranium concentrations in all samples were less than 15μg/L which was the limit given by World Health Organization(WHO).Conclusions The concentration of uranium in water sources was as follows:Liaoning>Shandong>Jiangsu>Zhejiang.The concentration of uranium in drinking water W88 maximal in Shandong Province and minimal in Zhejiang Province.
7.Estimation and application of uncertainty of measurement in detecting of hepatitis B virus DNA by method of fluorescence quantitative polymerase chain reaction
Wei-Feng SHEN ; Ren-Ye DING ; Qing-Ping YANG ; Ping-Yang SHAO ;
Chinese Journal of Laboratory Medicine 2001;0(02):-
Objective To estimate the uncertainty of measurement in detecting of hepatitis B virus DNA(HBV DNA)by method of fluorescence quantitative polymerase chain reaction(FQ-PCR),and discuss the application value.Methods The process of the detection of HBV DNA by FQ-PCR was analysed to confirm and simplify the sources of uncertainties of measurement,which were obtained by disposing the data of methodology validation,internal quality control(type A evaluation of uncertainty)and external quality assessment(type B evaluation of uncertainty);combined uncertainty and expanded uncertainty were obtained by statistical methods.Results The main sources of uncertainties of measurement were:precision within laboratory,precision between laboratory,method bias.The expanded uncertainty of HBV DNA by FQ-PCR was U=0.62(k=1.96,n=2).The uncertainty caused by method bias was found mostly.Conclusion Expanded uncertainty can be compared in different results of HBV DNA by FQ-PCR,and it provides guide significance for observing the cure effect of anti-HBV and choosing the concentration of quality control.
8.Effects of survivin gene siRNA on the growth of gastric cancer cell line
Shao-Chang JIA ; Chang-Qing SU ; Wei-Bing ZHANG ; Yue-Hua WANG ; Yong-Zhong YU ;
Chinese Journal of General Surgery 2000;0(12):-
Objective To construct an expression plasmid carrying the specific siRNA of survivin gene,and to evaluate its silencing effect on the expression of survivin gene and its inhibition effect on the growth of gastric cancer cells.Methods The specific siRNA of survivin gene was designed and synthesized,and an expression plasmid pAdGFP-siRNA was constructed.Gastric cancer cell line SGC-7901 was cuhured and transferred with pAdGFP-siRNA,then the silencing of survivin gene expression and the growth inhibition of cancer cell mediated by pAdGFP-siRNA were identified.Results The growth of gastric cancer cells was inhibited after transferring the pAdGFP-siRNA,with the inhibition rate of 68.2% compared to the control group.Immunohistochemistry showed that the specific siRNA markedly silenced the expression of survivin gene in cancer cells.Conclusions The overexpression of survivin gene in gastric cancer cells results in the high proliferation and the resistance to the chemo- and radio-therapy of the cancer cells.The specific siRNA can markedly silence the expression of survivin gene and inhibit the growth of cancer cells.
9.Dopamine transporter SPECT imaging of the peroral addictors of compound codeine phosphate solution
Tao-tao, SUN ; Shu, HU ; Shao-wei, JIA ; Qing, CHEN ; Rong, FAN
Chinese Journal of Nuclear Medicine 2010;30(6):379-382
Objective To study the damage to striatum in patients perorally addicted to compound codeine phosphate solution by using the brain dopamine transporter SPECT imaging. Methods Patients p erorally addicted to compound codeine phosphate solution ( n = 29 ) and addicted to heroin ( n = 27 ), as well as healthy volunteers (n = 31 ) were included in the study. Each of them underwent dopamine transporter (DAT) SPECT imaging with 99Tcm-2β-[N, N'-bis-( 2- mercaptoethyl ) ethylenediamino] methyl, 3β-(4-chlorophenyl)tropane (99Tcm-TRODAT-1). The striatum volume (V, cm3), mass (m, g) and radiactivity ratio (Ra) of striatum to whole brain were calculated using physio-mathematical modeling method.R esults Bilateral striatum of healthy volunteers showed typical "panda eyes" pattern and the distribution of DAT was uniform and symmetrical. Bilateral striatum of patients addicted to compound codeine phosphate showed impaired tracer uptake, similar to those addicted to heroin. The V, m and Ra of bilateral striatum of patients addicted to compound codeine phosphate were (23.68 ±4.94) cm3, (24.87 ±5.19) g and (5.01 ±0. 88 ) %, respectively, which were significantly lower than those of healthy controls: ( 35.39 ± 4.42 ) cm3,(37.16 ±4.64) g and (7.93 ±0.86)% (t = -9.69, -9.69, - 13.01, all P =0.000), but significantly higher than those addicted to heroin: ( 18.87 ± 4.66 ) cm3, ( 19.81 ± 4.90 ) g and (4.26 ± 1.02 ) % ( t =3.74, 3.74, 2.96, P = 0.000, 0.000, 0.005 ). Conclusion Long-term peroral intake of compound codeine phosphate solution may damage the function of cerebral striatum, which is someway similar to though less severe than, the impairment caused by heroin.
10.Determination by ICP-MS of uranium isotopic ratios in drinking water in the vicinity of nuclear power plants
Qing TIAN ; Yanqin JI ; Liangliang YIN ; Wei HUANG ; Xianzhang SHAO ; Baoming SHEN
Chinese Journal of Radiological Medicine and Protection 2013;(1):72-75
Objective To ascertain the uranium isotopic ratios in surface water samples around nuclear power plants.Methods Water samples were collected in Jiangsu,Shandong and Zhejiang provinces.An efficient separation procedure for the trace uranium concentrated from surface water by tributyl phosphate (TBP) was used.Inductively coupled plasma mass spectrometry (ICP-MS) was applied to determination of low abundance uranium isotopes.Results The 234 U/238 U isotope ratio varied from 4.575 × 10-5to 7.752 × 10-5 and 235U/238U from 7.273 × 10-3 to 7.639 × 10-3.Conclusions The 234U is enriched in the surface water.