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Objective:To set up an automatic gel permeation chromatography-solid phase extraction purification-ultra performance liquid chromatography-tandem mass spectrometry ( GPC-SPE-UPLC-MS/MS ) method for the quantitative determination of 14 carba-mates pesticide residues in Chinese herbal pieces. Methods:The samples were extracted by acetonitrile, and kept in constant volume with ethyl acetate-cyclohexane (1: 1, v/v). The extract was purified by GPC combined with amino solid phase extraction column (Carb/NH2). After UPLC gradient elution separation on an Agilent Poroshell 120EC-C18 column using acetonitrile-0. 1% formic acid as the mobile phase,the target pesticides were determined by tandem mass spectrometry in a multi-reaction monitoring ( MRM) mode. Results:The 14 kinds of carbamates pesticides had good linear relationships within the range of determination (r>0. 9990), and the detection limit was 0. 02-0. 35μg·kg-1 . When the spiked levels were 1, 10 and 50μg·L-1 , the recoveries were 74. 2%-108. 8%, and the RSD was 1. 25%-6. 73%(n=6). Conclusion:The method simplifies the pretreatment operation and shortens the analysis time with good selectivity and high sensitivity, which can be used for the determination of carbamates pesticide residues in Chinese herbal pieces.
RESUMO
Objective A method for quantitative determination of 16 kinds of organochlorine pesticide (OCPs) in aquatic prod-ucts by gas chromatography (GC)was established .Methods The sample was extracted by acetonitrile ,purified by Carb/NH2 ,and then determined by GC .Results The linear relations of 16 kinds of OCPs were good at 0 .05 - 1 .00 mg/L(r> 0 .998) .The limit of detection of OCPs was in the range of 0 .04 - 0 .31 μg /kg(S/N = 3) .When the standard levels were 50 ,100 ,200 μg /kg ,the recovery rates were 72 .6% - 115 .2% ,the relative standard deviations were 0 .6% - 7 .5% .Conclusion The method established in this stud-y is applied to the determination of 16 kinds of OCPs in real samples with satisfactory results .
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Objective To establish a method for quantitative determination of 17 kinds of organophosphates pesticides in vegeta‐bles by gas chromatography and mass spectrometry (GC‐MS) .Methods The sample was extracted by acetonitrile ,purified by the a‐mino solid phase extraction small column ,concentrated ,detected by GC‐MS .Then the ion scanning (SIM ) mode was selected to mo‐nitor the specific iron in target compound for conducting the quantitative analysis .Results 17 kinds of compound had good linearity in the limit of detection (LOD) of 0 .001 - 0 .02 mg /kg (S/N = 3) with a relative standard deviation of 1 .05% - 6 .81% ,and the re‐covery rate was 66 .4% - 99 .3% when with cap at 004 ,008 ,0 .40 mg/kg .Conclusion This method has good selection and high sensitivity ,and is suitable for the rapid determination of organophosphates pesticide residues in vegetables .
RESUMO
OBJECTIVE:To establish a method for simultaneous determination of the contents of Cu,Pb,As,Cr,Cd,Ba, Mn,Sb and Hg in Ganmaoling granule. METHODS:ICP-MS was conducted. The sample was handled by nitric acid microwave di-gestion system,the mass concnetration of 9 metal elements were determined by ICP-MS with Ge,In,Bi as internal standard and standard substance of test element standards. RF power was 1 100 W,sampling depth was 8 mm,carrier gas was argon(Ar)with high purity and flow rate was 1.0 L/min. RESULTS:All 9 elements had good linear range between mass concentration and ion peaks (r=0.999 1-0.999 9),detection limits were in the range of 0.3-6.0μg/L;RSDs of precision,stability and reproducibility tests were no more than 6.0%;average recoveries were in the range of 80.0%-113.5%,and RSDs were in 1.0%-4.5%. CONCLUSIONS:The method is simple,rapid and accurate,and can be used for the determination of 9 metal elements in Ganmaoling granule.