中藥材有機氯類農藥殘留之分析研究   全文下載

Determination of Organochlorine Pesticides in Crude Drugs

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（注入重覆性、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。1.0 ppm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 multiresidue method using gas chromatography (GC) and gas chromatography/ mass spectrometry (GC/MS) was developed for the determination of several organochlorine pesticides in three crude drugs: Astragali Radix (黃耆)、Zizyphi Sativae Fructus (大棗)、and Zingiberis Rhizoma (乾薑). The pesticides including α-BHC, β-BHC, γ-BHC, δ-BHC, 2,4'DDE, 4,4'-DDE, 2,4'-DDT and 4,4'-DDT were determined using a modified extraction and refining procedure, separated by a capillary column (DB-1, 0.25 μm, 0.25 mm x 30 M), observed with an electron capture detector (ECD), and confirmed by GC/MS if necessary. The precision and accuracy were satisfactory. Calibration graphs of eight pesticides were constructed in the range of 0.25- 2.0 μg/ml and their correlation coefficients (r) were in the range of 0.995 - 0.998. Recovery studies were performed at the 1.0 ppm spike level of each pesticide in these three crude drugs. Recovery rates were 66.4 - 98.0% for Astragali Radix, 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 detection of the pesticides were all below the 0.06 ppm level. Coefficients of variation ranged between 6.3 and 10.2%. This analysis method could be also applied to concentrated Chinese medicines."

A multiresidue method using gas chromatography (GC) and gas chromatography/ mass spectrometry (GC/MS) was developed for the determination of several organochlorine pesticides in three crude drugs: Astragali Radix (黃耆)、Zizyphi Sativae Fructus (大棗)、and Zingiberis Rhizoma (乾薑). The pesticides including α-BHC, β-BHC, γ-BHC, δ-BHC, 2,4'DDE, 4,4'-DDE, 2,4'-DDT and 4,4'-DDT were determined using a modified extraction and refining procedure, separated by a capillary column (DB-1, 0.25 µm, 0.25 mm x 30 M), observed with an electron capture detector (ECD), and confirmed by GC/MS if necessary. The precision and accuracy were satisfactory. Calibration graphs of eight pesticides were constructed in the range of 0.25- 2.0 µg/ml and their correlation coefficients (r) were in the range of 0.995 - 0.998. Recovery studies were performed at the 1.0 ppm spike level of each pesticide in these three crude drugs. Recovery rates were 66.4 - 98.0% for Astragali Radix, 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 detection of the pesticides were all below the 0.06 ppm level. Coefficients of variation ranged between 6.3 and 10.2%. This analysis method could be also applied to concentrated Chinese medicines.