分析科学学报
分析科學學報
분석과학학보
JOURNAL OF ANALYTICAL SCIENCE
2009年
5期
537-541
,共5页
微波辅助提取%中草药%有机磷农药%氨基甲酸酯农药
微波輔助提取%中草藥%有機燐農藥%氨基甲痠酯農藥
미파보조제취%중초약%유궤린농약%안기갑산지농약
Microwave-assisted extraction%Gas chromatography%Chinese herbal medicine%Organophosphorus pesticide%Carbamate pesticide
建立了中草药中有机磷和氨基甲酸酯类农药同时检测的气相色谱分析新方法.中药材试样依据正交实验的优化条件,用正己烷-丙酮(1∶4,V∶V)混合提取剂进行微波辅助提取,经弗罗里硅土和中性氧化铝混合层析柱净化后,采用HP-5毛细管柱分离,氮磷检测器同时检测中草药中15种有机磷和6种氨基甲酸酯类农药残留量.21种农药在0.01～1.0 mg/L的浓度范围内线性良好,线性相关系数为0.9950～1.000,检出限为0.002～0.01 mg/L.在0.05、0.2、0.5 mg/kg三个添加水平的平均回收率分别为75.11%～128.57%、75.85%～120.71%和76.43%～117.25%,相对标准偏差分别为 3.10%～10.58%、5.27%～9.94%和4.03%～9.03%.方法用于中草药中有机磷和氨基甲酸酯类农药残留的同时检测,结果良好.
建立瞭中草藥中有機燐和氨基甲痠酯類農藥同時檢測的氣相色譜分析新方法.中藥材試樣依據正交實驗的優化條件,用正己烷-丙酮(1∶4,V∶V)混閤提取劑進行微波輔助提取,經弗囉裏硅土和中性氧化鋁混閤層析柱淨化後,採用HP-5毛細管柱分離,氮燐檢測器同時檢測中草藥中15種有機燐和6種氨基甲痠酯類農藥殘留量.21種農藥在0.01～1.0 mg/L的濃度範圍內線性良好,線性相關繫數為0.9950～1.000,檢齣限為0.002～0.01 mg/L.在0.05、0.2、0.5 mg/kg三箇添加水平的平均迴收率分彆為75.11%～128.57%、75.85%～120.71%和76.43%～117.25%,相對標準偏差分彆為 3.10%～10.58%、5.27%～9.94%和4.03%～9.03%.方法用于中草藥中有機燐和氨基甲痠酯類農藥殘留的同時檢測,結果良好.
건립료중초약중유궤린화안기갑산지류농약동시검측적기상색보분석신방법.중약재시양의거정교실험적우화조건,용정기완-병동(1∶4,V∶V)혼합제취제진행미파보조제취,경불라리규토화중성양화려혼합층석주정화후,채용HP-5모세관주분리,담린검측기동시검측중초약중15충유궤린화6충안기갑산지류농약잔류량.21충농약재0.01～1.0 mg/L적농도범위내선성량호,선성상관계수위0.9950～1.000,검출한위0.002～0.01 mg/L.재0.05、0.2、0.5 mg/kg삼개첨가수평적평균회수솔분별위75.11%～128.57%、75.85%～120.71%화76.43%～117.25%,상대표준편차분별위 3.10%～10.58%、5.27%～9.94%화4.03%～9.03%.방법용우중초약중유궤린화안기갑산지류농약잔류적동시검측,결과량호.
A new method for the simultaneous determination of organophosphorus and carbamate pesticide residues in Chinese herbal medicines by gas chromatography has been proposed. Extraction conditions were optimized using orthogonal experimental design. The 15 organophosphorus and 6 carbamate pesticide residues in Chinese herbal medicine were extracted by microwave-assisted extraction with hexane-acetone (1∶4, V∶V) as slovent. The post-extraction organic phase was cleaned up by a column filled with florisil and neutral aluminum oxide. And the analytical screening was determined by gas chromatography using HP-5 capillary column equipped with nitrogen-phosphorus detector. The proposed method show a good linearity between analytical signal and analyte concentration in the range of 0.01～1.0 mg/L with the linear correlation coefficients of 0.9950～1.000 and limits of detection of 0.002～0.01 mg/L. The average recoveries obtained from samples spiked with standards at the concentration levels of 0.05 mg/kg; 0.2 mg/kg and 0.5 mg/kg were in the range of 75.11%～128.57%; 75.85%～120.71% and 76.43%～117.25%, respectively, with relative standard deviations of 3.10%～10.58%; 5.27%～9.94% and 4.03%～9.03%, respectively. A satisfactory result was obtained by the simultaneous determination of organophosphorus and carbamate pesticide residues in Chinese herbal medicines.
