篇名 | 中藥材有機氯類農藥殘留之分析研究 |
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卷期 | 7:2 |
並列篇名 | Determination of Organochlorine Pesticides in Crude Drugs |
作者 | 賴文苓 、 邵震茹 、 許世興 |
頁次 | 153-162 |
關鍵字 | 萃取精製法 、 農藥 、 殘留 、 Crude drug 、 Organochlorine pesticides 、 Multiresidue 、 MEDLINE 、 Scopus 、 SCIE |
出刊日期 | 199906 |
本研究係採用稍加修飾之萃取精製法,於黃耆、大棗及乾薑三種藥材中,以氣相層析法(GC)進行殘留農藥α-BHC、β-BHC、γ-BHC、δ-BHC、2,4'-DDE、4,4'-DDE、2,4'-DDT及4,4'-DDT八種有機氯類農藥之偵測,必要時,以氣相層析/質譜法(GC/MS)作確認;並進行該分析方法之確效,包括精密度(注入重覆、日內及日間相對標準偏差)、線性範圍、準確度(添加回收率)和檢測、定量極限。其中八種農藥溶液之同日內精密度變異係數均小於5%。八種有機氯類農藥在0.25-2.0μg/mL濃度範圍內之標準曲線均呈良好線性關係。1.0ppm添加量之回收試驗結果,除2,4'-DDE、4,4'-DDE、2,4'-DDT及4,4'-DDT受乾薑樣品基質干擾,無法測定外,黃耆介於66.4-98.0%之間,大棗介於36.7-86.9%之間,乾薑介於31.1-109.7%之間,變異係數則介於2.3-4.9%。八種農藥在三類藥材中之最低檢測極限可低至0.06 ppm以下,變異係數介於6.3-10.2%之間。此檢驗方法亦適用於市售中藥濃縮製劑。
A multi-residue method using gas chromatography (GC) and gas chromatography!mass spectrometry (GC/MS) was developed for the determination of severalorganochlorine pesticides in three crude drugs: Astragali Radix (黃耆), ZizyphiSativae Fructus (大棗), and Zingiberis Rhizoma (乾薑). The pesticides including v-BHC, β-BHC, γ-BHC, δ-BHC, 2,4'-DDE, 4,4'-DDE, 2,4'-DDT and 4,4'-DDT weredetermined using a modified extraction and refining procedure, separated by acapillary column DB-1, 0.25 μm, 0.25 mm * 30 M), observed with an electron capturedetector (ECD). amid confirmed by GC/MS if necessary. The precision and accuracy weresatisfactory. Calibration graphs of eight pesticides were constructed in the rangeof 0.25-2.0 - μg/ml and their correlation coefficients (r) were in the range of0.995-0.998. - Recovery studies were performed at the 1.0 ppm spike level of eachpesticide in these three crude drugs. Recovery rates were 66.4-98.0% for AstragaliRadix. 36.7-86.9% for Zizyphi Sativae Fructus, and 31.1-109.7% for Zingiberis Rhizoma.Coefficients of variation were between 2.3 and 4.9%. The estimated limits of detectionof the pesticides were all below the 0.06 ppm level. Coefficients of variation rangedbetween 6.3 and 10.2%. This analysis method could be also applied to concentratedChinese medicines.