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本研究係以固相萃取(Solid-phase extraction, SPE)操作，配合液相層析建立一套多重殘留之分析方法，可同時檢測6 種常見的蔬菜（芥藍、結球白菜和茄子）及水果（柳橙、木瓜和草莓）中四種巨環內酯類農藥及其代謝產物之微量殘留。利用氰甲烷及醋酸銨緩衝溶液(10 mM, pH 4.0)(90:10, v/v)萃取樣品中殘留農藥，以NH2固相萃取匣作爲凈化，並以逆相高效能液相層析儀及C18分離管柱進行檢液中分析物分離，以紫外光波長250 nm偵測之。分析方法確效試驗，標準劑添加濃度爲2、20 及100μg/mL 三種濃度（添加體積爲1.5 mL，樣品相當於添加濃度分別爲0.15、1.5 及7.5 μg/g），方法試驗結果，平均回收率介於75-117% 之間，相對標準偏差介於0.4-13.3% 之間。顯示本試驗方法之準確度(accuracy)及精密度(precision)均符合歐盟之農藥殘留分析品管規範(SANCO/2007/3131)，即平均回收率(mean recovery)介於70-120% 之間，及相對標準偏差(relative standard deviation, RSD)不大於20%。方法偵測極限(method LOD)介於0.01至0.03 μg/g之間。本方法分析效能可靠、操作簡易有效率，可用時檢測農產品中四種巨環內酯類農藥及其代謝產物。

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 Rhi

The HPLC analytical method and manufacturing process of Hwan-Shio-DanSoftgel were developed in this study. First, Chinese crude drugs contained inHwan-Shio-Dan were purchased and selected. They were then processed by adecoction extractor, centrifugal filter, centrifugal thin-film vacuumedevaporation machine, and spray dryer. Finally, the dry powder from the spraydryer was homogenized with an oil substance and sealed in a softgel form. At thesame time, a HPLC analytical method for loganin and β asarone constituted inHwan-Shio-Dan was developed to evaluate the stability of Hwan-Shio-Dan softgel.The results showed that the appearance of Hwan-Shio-Dan softgel was good.Although one of the marker substances, loganin, slowly decayed with time and thetendency of the degradation became obvious with an increase in the storagetemperature, the other maker substance, β-asarone, was quite stable during theaccelerated stability study.