1.Determination of Three Sulfonamides Residues in Animal Derived Food by UPLC-MS/MS
Xingcui LI ; Baoming LI ; Yaping TIAN
China Pharmacist 2015;(1):38-40,41
Objective:To establish a determination method for sulfadoxine, sulfathiazole and sulfadiazine in animal derived prod-ucts by ultra-performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS) . Methods:Trichloroacetic acid and ace-tonitrile were used in the extraction and removal of proteins. A Waters Acquity UPLC BEH C18 (100 mm × 2. 1 mm,1. 7 μm) column was used as the separation column. The mobile phase was 0. 1% formic acid in water-methanol with gradient elution. The three sulfona-mides residues were detected with multiple reaction monitoring( MRM) mode in multi-period. Results:Under the conditions,the linear range of sulfadoxine, sulfathiazole and sulfadiazine was 1. 0-200. 0 ng·ml-1 ,the linear correlation coefficient was above 0. 99,the re-covery was more than 70%,the detection limit was 0. 5 ng·ml-1 , and the quantification limit was 1. 0 ng·ml-1 . Conclusion: The sample preparation method is simple and fast, and the method can be used to analyze sulfadoxine, sulfathiazole and sulfadiazine in ani-mal derived food efficiently and sensitively.
2.Relationship between TGF ?1 expression and apoptosis in hepatocytes during acute hemorrhagic necrotic pancreatitis
Haiyan LI ; Ruifen CHEN ; Guozhen LIU ; Jue WANG ; Xingcui WANG
Chinese Journal of Pathophysiology 2000;0(07):-
AIM: To observe the expression of TGF ?1 in hepatocytes during acute hemorrhagic and necrotic pancreatitis (AHNP) and to study the relationship between TGF ?1 and apoptosis in hepatocytes. METHODS: AHNP was induced in 40 rats weighting 260-280 g by intraductal administration of 5% sodium taurocholate. The pathologic morphologic changes of liver and pancreas were observed under light microscope. The hepatocyte apoptosis was examined through TdT (terminal deoxynucleotidyl transferase) mediated dUTP nick end labeling (TUNEL) and the expression of TGF ?1 in hepatocytes was analyzed through immunohistochemistry. RESULTS: The liver injuries were found at 3 h after the inducement. These changes were aggravated with the development of the disease. The apoptotic hepatocytes were found after 3 h (P
3.Establishment and evaluation of the review criteria of automatic urine analysis workstations
Junlong MA ; Yujing LU ; Xingcui LI ; Shengjiang WANG ; Jie LI ; Xiaojing MA ; Yulong CONG
Chinese Journal of Laboratory Medicine 2012;35(9):810-814
ObjectiveTo establish the proper review rules for the microscopic screening of urine samples tested by automatic urinalysis work station which is composed of LabUMat urine dry chemical analyzer and Urised urine sedimental analyzer.Methods The paired comparison was used to analyze the results tested by microscopy and Urised.A total of 2015 random urine samples were enrolled to establish and validate review rules.All the samples were collected from the inpatients and ontpatients of General Hospital of the People's Liberation Army from May to November 2011 and tested by urinalysis work station.2015 urine samples were firstly tested by urinalysis work station,including both urine dry chemical analyzer and urine sediments analyzer.Then each urine sample was examined microscopically by two technicians-in-charge using double-blind method.The average results from the two technicians were used as review results.Compared with review results,we set up the review rules and evaluated the Irue positive rate,false positive rate,true negative rate,false negative rate (omission diagnostic rate) and review rate.According to different test methods by automatic urinalysis work station,four microscopic review protocols were defined:( 1 ) Protocol 1:based on chemistry results only,microscopy review was performed when any of WBC,RBC,PRO and NIT was positive; (2) Protocol 2:based on urine sedimental analysis only,microscopy review was performed when any of WBC,RBC and CAST count was over upper limit of the reference range ; (3) Protocol 3:if any of BLD vs.RBC,LEU vs.WBC was different between two systems,or quantitative results had two or more than two gradient differences,microscopy review was performed; (4) Protocol 4:if any of BLD vs.RBC,LEU vs.WBC was different between two systems,or CAST was over upper limit of the reference range,or alam appeared,microscopic review was performed.300 randomly selected urine samples were tested to validate the review rules.Omission diagnostic rate and review rate were used to evaluate the rules.Results According to our review rules,the positive samples rate was 41.14% (829/2015) and the negative rate was 58.86% ( 1186/2015 ) ; Positive samples were composed of RBC (50.30%),WBC (53.32%) and CAST (3.74%).The review rates of four protocols were 42.93% (865/2015),39.70% (810/2015),29.58%(596/2015),18.91% (381/2015 ),respectively.The false negative rates (omission diagnostic rates) were 6.36% (128/2015),4.42% (89/2015),1.34% (27/2015)and 1.04% (21/2015)respectively.Protocol 4 was selected as an ideal plan.Additional 300 urine samples were tested using protocol 4 in order to confirm the review rule.The review rate,consistency rate,true positive rate,false positive rate,true negative rate,omission diagnostic rate were 19.67% (59/300),91.67% (275/300),35.67% (107/300),7.67%(23/300),56.00% (168/300),0.67% (2/300),respectively.After image review revised,the review rate was 8.67% (26/300).ConclusionThe review rules established by our research for Urinalysis Work Station can find the abnormal urine samples effectively and exactly and can reduce the workload significantly.(Chin J Lab Med,2012,35:810-814)
4.Chemical constituents from Salvia przewalskii Maxim.
Lixin YANG ; Xingcui LI ; Chao LIU ; Lei XIAO ; Dehua QIN ; Ruoyun CHEN
Acta Pharmaceutica Sinica 2011;46(7):818-21
The investigation on Salvia przewalskii Maxim was carried out to find the relationship of the constituents and their pharmacological activities. The isolation and purification were performed by various chromatographies such as silica gel, Sephadex LH-20, RP-C18 column chromatography, etc. Further investigation on the fraction of the 95% ethanol extract of Salvia przewalskii Maxim yielded przewalskin Y-1 (1), anhydride of tanshinone-II A (2), sugiol (3), epicryptoacetalide (4), cryptoacetalide (5), arucadiol (6), 1-dehydromiltirone (7), miltirone (8), cryptotanshinone (9), tanshinone II A (10) and isotanshinone-I (11). Their structures were elucidated by the spectral analysis such as NMR (Nuclear Magnetic Resonance) and MS (Mass Spectrometry). Compound 1 is a new compound. Compounds 4 and 5 are mirror isomers (1 : 3). Compounds 4, 5, 6, 8, 11 were isolated from Salvia przewalskii Maxim for the first time.
5.Chemical constituents of Acacia catechu.
Xingcui LI ; Hongqing WANG ; Chao LIU ; Ruoyun CHEN
China Journal of Chinese Materia Medica 2010;35(11):1425-1427
OBJECTIVETo study the chemical constituents of Chinese medicine Acacia catechu.
METHODIsolation and purification were carried out on normal phase silica gel, Sephadex LH-20, ODS column chromatography etc. Constituents were identified by physicochemical properties and spectral analysis.
RESULTTwelve compounds were identified as 4-hydroxybenzoic acid( 1), kaempferol (2), quercetin (3), 3,4',7-trihydroxyl-3', 5-dimethoxyflavone (4), catechin (5), epicatechin (6), afzelechin (7), epiafzelechin (8), mesquitol(9), ophioglonin (10), aromadendrin (11), and phenol (12).
CONCLUSIONCompounds 7, 12 were isolated from A. catechu for the first time, and compounds 4, 9-11 were isolated from the genus Acacia for the first time.
Acacia ; chemistry ; Plant Extracts ; analysis ; isolation & purification
6.Effects of l-tetrahydropalmatine on different stages of conditioned place preference in ketamine dependent rats and the mechanism of DA
Yan DU ; Xingcui GAO ; Hongliang SU ; Yujin WANG ; Li DU ; Keming YUN
Chinese Journal of Forensic Medicine 2024;39(1):50-54
Objective To observe the effects of Levo-tetrahydropalmatine(l-THP)on the expression,regression and relapse of conditioned place preference(CPP)in ketamine induced rats,and to detect the content of dopamine(DA)in the striatum(caudate putamen,CPu)of the rat brain at different time points.Methods Ketamine addiction rat model was established by CPP.The effects of l-THP on the expression,regression and relapse of ketamine induced rat CPP were investigated using CPP score as the index.The content of DA in CPu of rats was determined by ultra-performance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS)after ketamine administration and l-THP intervention at 30 min,60 min,90 min,120 min and 150 min.Results It indicated that 1-THP could decrease the expression of CPP in ketamine induced rats,promote the process of CPP resolution and inhibit the process of relapse.In addition,l-THP combined with ketamine administration significantly inhibited the ketamine-induced increase in DA content in the CPu of the rats.Conclusion The mechanism of l-THP inhibiting the reward effect of ketamine may be related to blocking DA receptors and reducing the release of DA neurotransmitters.l-THP has potential implications for the treatment of ketamine addiction.