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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.
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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)
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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.
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<p><b>OBJECTIVE</b>To study the chemical constituents of Chinese medicine Acacia catechu.</p><p><b>METHOD</b>Isolation 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.</p><p><b>RESULT</b>Twelve 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).</p><p><b>CONCLUSION</b>Compounds 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.</p>