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ABSTRACT: A new method was developed for the rapid screening and confirmation analysis of barbital, amobarbital and phenobarbital residues in pork by gas chromatography-tandem mass spectrometry (GC/MS/MS) with ion trap MSD. The residual barbiturates in pork were extracted by ultrasonic extraction, cleaned up on a multiwalled carbon nanotubes (MWCNTs) packed solid phase extraction (SPE) cartridge and applied acetone-ethyl acetate (3:7, v/v) mixture as eluting solvent and derivatized with CH3I under microwave irradiation. The methylated barbiturates were separated on a TR-5MS capillary column and detected with an ion trap mass detector. Electron impact ion source (EI) operating MS/MS mode was adopted for identification and external standard method was employed for quantification. One precursor ion m/z 169 was selected for analysis of barbital and amobarbital and m/z 232 was selected for phenobarbital. The product ions were obtained under 1.0 V excitation voltage. Good linearities (linear coefficient R > 0.99) were obtained at the range of 0.5-50 microg kg(-1). Limit of detection (LOD) of barbital was 0.2 microg kg(-1) and that of amobarbital and phenobarbital were both 0.1 microg kg(-1) (S/N > or = 3). Limit of quantification (LOQ) was 0.5 microg kg(-1) for three barbiturates (S/N > or = 10). Satisfying recoveries ranging from 75% to 96% of the three barbiturates spiked in pork were obtained, with relative standard deviations (R.S.D.) in the range of 2.1-7.8%.
Analytica chimica acta 04/2007; 586(1-2):399-406. · 4.31 Impact Factor
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ABSTRACT: A solid-phase extraction (SPE)/GC-MS method using multiwalled carbon nanotubes (MWCNTs) was developed for the determination of four benzodiazepine residues including diazepam, estazolam, alprazolam and triazolam in pork. The analytes were extracted by ultrasonic assistant extraction using acetonitrile, concentrated and purified by MWCNTs packed cartridge, and determined by GC-MS. Ultrasonic extraction conditions, which included temperature, time, power, and solvent volume, were optimized. Comparative studies showed that MWCNTs were superior to C18 for the adsorption of drugs. Parameters influencing SPE efficiency, such as sample amounts, variety and volume of the eluent, were also optimized. Electron ionization (EI) operating in time program-selected ion monitoring mode (SIM) was used for GC-MS identification. The analytes were quantified with external standard calibration curve method. Lower limit of detection and quantification was obtained by the new method. Linear calibration curves were obtained in the concentration range from 10 ng/mL to 500 ng/mL for diazepam and from 20 ng/mL to 1000 ng/mL for estazolam, alprazolam and triazolam with calibration coefficients of 0.99 and above. The average recoveries for the four benzodiazepines spiked in pork were 75% to 104% and their relative standard deviations were between 1.3% and 10%. The limits of detection were 2 microg/kg for diazepam and 5 microg/kg for estazolam, alprazolam and triazolam in pork, respectively.
Journal of Chromatography 01/2007; 1136(1):99-105. · 4.53 Impact Factor
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ABSTRACT: A new method was developed for the rapid extraction and unequivocal determination of barbital, amobarbital and phenobarbital residues in pork. The isolation of the analytes from pork samples was accomplished by utilizing an accelerated solvent extractor ASE 300. The procedure was automatically carried out in series for fat removing and extraction, respectively with n-hexane and acetonitrile pressurized constantly at 10.3 MPa for 30 min. After evaporation, the extracts were cleaned up on a C(18) solid phase extraction (SPE) cartridge and the barbiturates were eluted with hexane-ethyl acetate (7:3), evaporated on a rotary evaporator and derivatized with CH(3)I. The methylated barbiturates were separated on a HP-5MS capillary column and detected with a mass detector. Electron impact ion source (EI) operating in time program-selected ion monitoring mode (SIM) was used for identification and external standard method was used for quantification. Good linearity was obtained in the range from 0.5 microg/kg to 25 microg/kg. Average recoveries of the three barbiturates spiked in pork ranged from 84.0% to 103.0%, with relative standard deviations from 1.6% to 12%. The limit of detection (LOD) was 0.5 microg/kg for the three barbiturates (S/N>or=3). The quantification limit (LOQ) was 1 microg/kg for the three barbiturates (S/N>or=10).
Journal of Chromatography B 08/2006; 840(2):139-45. · 2.89 Impact Factor
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ABSTRACT: A rapid, sensitive and accurate method has been developed for the determination of seventeen 2, 3, 7, 8-substituted congeners of polychlorinated dibenzo-p-dioxins and dibenzo-furans (PCDD/Fs) in sediment using isotope dilution high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). Dibenzo-p-dioxins and dibenzo-furans were extracted from samples by accelerated solvent extraction (ASE) and then purified by fluid management systems (FMS) with silica column, alumina column and carbon column. Confirmation and quantitative analysis at pg/g level of PCDD/Fs were performed by HRGC/HRMS using voltage selective ion record (VSIR) mode. Recoveries of fifteen isotopically labeled compound solutions (LCS) and the precision and recovery standards (PAR) were found to be in the range of 49.8% -85.3% and 93.2% - 113.8%, respectively. The detection limits of the method for both 2, 3, 7, 8-tetrachloro-dibenzo-furan (TCDF) and 2, 3, 7, 8-tetrachloro-dibenzo-p-dioxin (TCDD) were determined to be 0.1 pg/g. This method not only meets the requirements of international standards, but also shortens analysis time from 2 weeks to 2 days.
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 08/2006; 24(4):347-50.
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ABSTRACT: A method was developed for the simultaneous determination of chloramphenicol (CAP), thiamphenicol (TAP), and florfenicol (FF) residues in animal tissues using gas chromatography/mass spectrometry (GC/MS) with chemical ionization source in negative mode. The homogenized samples were extracted with ethyl acetate and the extracts were partitioned with n-hexane to remove lipids. Further cleanup was performed on a florisil cartridge and the purified samples were derivatized with Sylon BFT [N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA)-trimethylchlorosilane (TMCS), 99: 1, v/v] in toluene. Meta-nitrochloramphenicol (m-CAP) was used as the internal standard for the determination. Selected ion monitoring (SIM) was used for detection, ions were chosen, respectively, for the monitoring at m/z 432, 466, 468, 470 for m-CAP, m/z 376, 378, 466, 468 for CAP, m/z 409, 411, 499, 501 for TAP, and m/z 339, 341, 429, 431 for FF. Quantitative ions were selected at m/z 466 for CAP and m-CAP, at m/z 339 for FF and at m/z 409 for TAP. The detection limits were 0.03 microg/kg for CAP, 0.2 microg/kg for FF and TAP. The correlation coefficients were above 0.99 for the calibration curves of the medicines. The linear ranges were 0.1 - 8.0 microg/kg for CAP and 0.2 - 4.0 microg/kg for FF and TAP. The reproducibilities of the compounds within a batch were 5.5%, 10.4%, and 8.8% for CAP, FF, and TAP respectively, while the corresponding values between the batches were 7.4%, 20.7%, and 19.1%. The recoveries were 80.0% - 111.5%, and the relative standard deviations were 1.2% - 15.4%. The method is applicable for detection of the residues in animal derived food, such as pork, poultry and aquatic products.
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 02/2006; 24(1):14-8.
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ABSTRACT: A method was developed for the determination of acrylamide in fried starchy foods using isotope dilution gas chromatograpy-selected mass spectrometry (GC-MS). The acrylamide was extracted from samples by water, then centrifuged and cleaned up by a column of graphitized carbon black. Acrylamide was derivatized through bromination at low pH and low temperature and determined by GC-MS. With the aid of the 13C-substituted acrylamide internal standard, the mass spectrum in GC-MS was interpreted, and the content of acrylamide was measured. The limit of quantitative detection (S/N > 10) was 5 microg/kg and the recovery was in the range of 90%-105% and relative standard deviation is 6.3%. The levels of acrylamide in some fried foodstuffs such as French fries was surveyed using the method. French fries were found to contain 278-4518 microg/kg acrylamide. It means that the content of acrylamide in French fries is 10,000 times higher than the drinking water guideline of World Health Organization for acrylamide.
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 05/2005; 23(3):312-4.
