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Rapid gas chromatography with flame photometric detection of multiple organophosphorus pesticides in Salvia miltiorrhizae after ultrasonication assisted one-step extraction

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单位: [1]Chinese Acad Med Sci, Key Lab Bioact Subst & Resources Utilizat Chinese, Minist Educ, Inst Med Plant Dev, Beijing 100193, Peoples R China [2]Peking Union Med Coll, Beijing 100193, Peoples R China [3]Jinzhou Med Univ, Coll Pharm, Jinzhou 121001, Peoples R China [4]Jilin Agr Univ, Coll Tradit Chinese Med, Changchun 130118, Jilin, Peoples R China [5]Shimadzu Enterprise Management China Ltd, Beijing 100020, Peoples R China [6]Capital Med Univ, Beijing Friendship Hosp, Dept Pharm, Beijing 100050, Peoples R China
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关键词: Organophosphorus pesticides Multi-residues determination Salvia miltiorrhizae Ultrasonication assisted one-step extraction GC-FPD

摘要:
A simple and rapid gas chromatography-flame photometric detection (GC-FPD) method was developed for the determination of 12 organophosphorus pesticides (OPPs) in Salvia miltiorrhizae by using ultrasonication assisted one-step extraction (USAE) without any clean-up steps. Some crucial parameters such as type of extraction solvent were optimized to improve the method performance for trace analysis. Any clean-up steps were negligent as no interferences were detected in the GC-FPD chromatograms for sensitive detection. Under the optimized conditions, limits of detection (LODs) and quantitation (LOQs) for all pesticides were in the range of 0.001-0.002 mg/kg and 0.002-0.01 mg/kg and 0.002-0.01 mg/kg, respectively, which were all below the regulatory maximum residue limits suggested. RSDs for method precision (intra- and inter-day variations) were lower than 6.8% in approval with international regulations. Average recovery rates for all pesticides at three fortification levels (0.5, 1.0 and 5.0 mg/kg) were in the range of 71.2-101.0% with relative standard deviations (RSDs) < 13%. The developed method was evaluated for its feasibility in the simultaneous pre-concentration and determination of 12 OPPs in 32 batches of real S. miltiorrhizae samples. Only one pesticide (dimethoate) out of the 12 targets was simultaneously detected in four samples at concentrations of 0.016-0.02 mg/kg. Dichlorvos and omethoate were found in the same sample from Sichuan province at 0.004 and 0.027 mg/kg, respectively. Malathion and monocrotophos were determined in the other two samples at 0.014 and 0.028 mg/kg, respectively. All the positive samples were confirmed by LC MS/MS. The simple, reliable and rapid USAE-GC-FPD method with many advantages over traditional techniques would be preferred for trace analysis of multiple pesticides in more complex matrices.

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出版当年[2016]版:
大类 | 3 区 医学
小类 | 3 区 生化研究方法 3 区 分析化学
最新[2025]版:
大类 | 3 区 医学
小类 | 3 区 生化研究方法 3 区 分析化学
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出版当年[2015]版:
Q2 BIOCHEMICAL RESEARCH METHODS Q2 CHEMISTRY, ANALYTICAL
最新[2023]版:
Q2 BIOCHEMICAL RESEARCH METHODS Q2 CHEMISTRY, ANALYTICAL

影响因子: 最新[2023版] 最新五年平均[2021-2025] 出版当年[2015版] 出版当年五年平均[2011-2015] 出版前一年[2014版] 出版后一年[2016版]

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第一作者单位: [1]Chinese Acad Med Sci, Key Lab Bioact Subst & Resources Utilizat Chinese, Minist Educ, Inst Med Plant Dev, Beijing 100193, Peoples R China [2]Peking Union Med Coll, Beijing 100193, Peoples R China [3]Jinzhou Med Univ, Coll Pharm, Jinzhou 121001, Peoples R China
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通讯机构: [1]Chinese Acad Med Sci, Key Lab Bioact Subst & Resources Utilizat Chinese, Minist Educ, Inst Med Plant Dev, Beijing 100193, Peoples R China [2]Peking Union Med Coll, Beijing 100193, Peoples R China
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