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<p><b>OBJECTIVE</b>To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides.</p><p><b>METHODS</b>After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode.</p><p><b>RESULTS</b>The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%.</p><p><b>CONCLUSION</b>This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.</p>
Assuntos
Humanos , Calibragem , Carbamatos , Urina , Cromatografia Líquida de Alta Pressão , Praguicidas , Urina , Espectrometria de Massas em TandemRESUMO
A method based on HPLC-ICP-MS was established to separate the reaction products of ( ethylenediamine) palladium(Ⅱ) chloride([Pd ( en ) Cl2])and 5’-deoxyguanylic acid ( 5’-dGMP). Two reaction products were detected at pH 8. 0 with 25 mmol/L phosphate buffer solution as chromatography eluent. One was the main product with HPLC retention time of 2. 8 min, the other product’s retention time was 3.2 min. According to ESI-MS(MS/MS) study, m/z=510, 511, 512, 514, 516[M+1]+ parent ions ( abundances same to palladium isotopes) were detected. Further analysis showed that the main product was[Pd( en) ( N1-5’-dGMP) ]. However the other product was hardly to be detected by ESI-MS. By using HPLC-DAD and HPLC-ICP-MS, we found that the two reaction products had the same UV absorption spectra and palladium percentage content. Combined with other groups’research, the other reaction product was deduced as dimmer, trimer or tetramer form of[Pd( en) ( N1-5’-dGMP) ]. Further study revealed that[Pd( en) ( N1-5’-dGMP) ] was easily formed in acid solution while its polymer form was generated in alkaline solution. At pH 6. 0, [Pd(en)(N1-5’-dGMP)] was formed within 12 hours with good stability. Research also revealed that the total amount of two reaction products declined as reaction pH climbed.
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A novel method was developed for the determination of the 15+1 European priority polycyclic aromatic hydrocarbons in edible oil by online solid-phase extraction coupled with high performance liquid chromatography-ultraviolet/ fluorescence detection ( online-SPE-HPLC-UV/FL-D ) . The edible oil samples were diluted with isopropyl alcohol, and then filtered. The online extraction was performed on a solid phase extraction ChromSpher Pi column (80 mmí3 mm) and the separation was carried out on a C18 reversed-phase PAH column (250 mmí4. 6 mm i. d, 5μm) using ultraviolet detection at 220 nm and fluorescence detection. Isopropyl alcohol, acetonitrile and water were served as mobile phase in gradient elution. The results showed good linearity for the 15+1 polycyclic aromatic hydrocarbons with all the correlation coefficients (R2)>0. 99. The limits of detection ( LODs ) were between 0. 03 and 12. 23 μg/kg. The recoveries of the sixteen components in the three levels of spiked samples were in the range of 65 . 3%-110 . 5% with the relative standard deviation (RSD, n=6) from 0. 1% to 9. 8%.
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<p><b>OBJECTIVE</b>To establish a method for simultaneously determining the urinary concentrations of 8-hydroxy-2'-deoxyguanosine (8-OHdG), trans, trans-muconic acid (tt-MA), and S-phenylmercapturic acid (S-PMA) in subjects exposed to benzene.</p><p><b>METHODS</b>After being purified by a solid-phase extraction column, the urine samples were transferred to a liquid chromatography-mass spectrometry system, and the concentrations of 8-OHdG, tt-MA, and S-PMA were determined by external standard method. A C18 reversed-phase column was used as the chromatographic column, and methanol/acidic ammonium formate solution was used as the mobile phase for gradient elution. The mass spectrometer was operated in a multi-reaction monitoring mode.</p><p><b>RESULTS</b>For tt-MA, the calibration curves were linear in the range of 10-1000 µg/L, and the recovery rates were over 90% (relative standard deviation (RSD) < 3%) at spiked levels of 50 µg/L and 500 µg/L. For S-PMA and 8-OHdG, the calibration curves were linear in the range of 1-100 µg/L, and the recovery rates were over 85% (RSD < 5%) at spiked levels of 5 µg/L and 50 µg/L.</p><p><b>CONCLUSION</b>This determination method meets the requirement of Biological materials-</p><p><b>METHODS</b>of monitoring-Guide of development (WS/T 68-1996) and can be used for simultaneous determination of 8-OHdG, tt-MA, and S-PMA in urine.</p>
Assuntos
Humanos , Acetilcisteína , Urina , Benzeno , Intoxicação , Cromatografia Líquida , Métodos , Desoxiguanosina , Urina , Espectrometria de Massas , Exposição Ocupacional , Ácido Sórbico , MetabolismoRESUMO
AstudyofPt-metabolitesfromanewanti-hepatomadrugmiriplatinwasimportanttomiriplatin's pharmacology research. Therefore, a method based on size exclusion chromatography-inductively coupled plasma mass spectrometry ( SEC-ICP-MS) was developed to study miriplatin and its Pt-metabolites in Beagle dog plasma. This method could be used to study total platinum concentration half-quantitatively. Compared with traditional ICP-MS direct determination, data acquired from this SEC-ICP-MS method were almost the same. By using BioSep-s2000 column, 25 mmol/L of pH 7. 2 phosphate buffer as eluent, and Pt-195 as detecting isotope, we discovered miriplatin with its four Pt-metabolites in dog plasma after intra-hepatic artery administration. The main Pt-metabolite was m2 , which associated with plasma proteins. Miriplatin in plasma did not bind with plasma proteins. According to calculation, the ratio of miriplatin/m2 first decreased rapidly, and then slowly increased to its second climax, finally slowly decreased.
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A method for the simultaneous determination of 34 pesticides in sunflower oil, soybean oil and corn oil was developed. The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry ( GPC-GC-MS ) . The linear range was from 0 . 01 to 0 . 2 mg/L with a good correlation coefficients ( r≥0. 9913). The average recoveries of 31 pesticides (except p,p′-DDE, p,p′-DDD, p,p′-DDT. For detail, please reference to section 3 . 6 ) ranged from 70 . 3% to 115 . 4%, 69 . 5% to 112 . 6% and 70 . 2% to 116 . 1%spiked at 0. 05 μg/g and 0. 1 μg/g with the relative standard deviations (RSDs, n=6) less than 13. 3%, 13. 5% and 12. 1% in sunflower oil, soybean oil and corn oil samples, respectively. The LODs of this method ranged from 0. 0692 to 2. 28, 0. 0559 to 2. 01 and 0. 0584 to 2. 14μg/kg (S/N=3) in sunflower oil, soybean oil and corn oil samples respectively. The convenient operation and versatility of this method are suitable for the fast screening and detection of 34 pesticide residues in sunflower oil, soybean oil and corn oil.
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Objective To establish an ultra performance liquid chromatography method for the determination of 7 kinds of antibiotics(minocycline hydrochloride,ox tetracycline,tetracycline hydrochloride,chlortetracycline hydrochloride,doxycycline hydrochloride,chloramphenicol,metronidazole) in anti-acne cosmetics.Methods Seven kinds of antibiotics were separated on a Waters UPLC BEH C18 column by gradient elution using A(methanol/acetonitrile = 1/2) and B(1% formic acid aqueous solution) as the mobile phase at a flow rate of 0.2 ml/min,with the detection wavelength of 268 nm.Results The detection limits were 0.3-0.5 ng,the calibration curves were linear in the range of 2-100 ng(1-50 mg/L),the precision was not more than 4.8% and the rate of recovery were 82.5%-105.6%.Conclusion The method established in the present paper is rapid,sensitive and suitable for the determination of 7 kinds of antibiotics in anti-acne cosmetics.