可移除性衍生之液相層析法分析藥酒中微量甲醇含量   全文下載

A Removable Derivatization HPLC for Analysis of Methanol in Chinese Liquor Medicine

本研究建立了一個可直接在高含水量且成分複雜之檢品中進行衍生而偵測微量甲醇的高效能液相層析法（HPLC）。以4-[N-methyl, N-（1-naphthylmethyl）]-amino-4-oxobutanoic acid （NAOB）, 4-dimethylaminopyridine （DMAP）和1-ethyl-3-（3-dimethylaminopropyl） carbodiimide hydrochloride （EDC）在溫和的條件下，將水溶液檢品之甲醇順利地進行衍生反應。反應液衍生後可用鹼洗、酸洗來移除有機層中過量的試劑及其他可被酸鹼移除之干擾物質。並對影響衍生反應之諸多因素皆詳加探討，找出最適當的衍生條件。應用此法於五種市售藥酒（乙醇含量8 ~ 55%，v／v）中甲醇含量之檢測，其結果為2 .20 × 10-4 ~ 3.28 × 10-3% （v／v），皆合乎甲醇含量之衛生標準（<0.1%，v／v）。"

A high performance liquid chromatography (HPLC) method for the determination of trace methanol in high water content sample has been established. Using 4-[N-methyl, N-(1-naphthylmethyl)]-amino-4-oxobutanoic acid (NAOB), 4-dimethylaminopyridine (DMAP) and 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) under a mild condition, the derivatization of methanol in aqueous solution was smoothly carried out before HPLC analysis. After derivatization, acidic or basic interfering substances and excess reagents can be easily removed from organic layer by simple acid-base shake-out. The condition for optimal derivatization of methanol in aqueous solution was established and applicable to the analysis of commercial Chinese liquor medicine (ethanol content 8~55%, v/v), the range of trace methanol in the above samples was 2.20 × 10-4~ 3.28 × 10-3% (v/v). The result showed that methanol contents in all samples were below regulation standard (< 0.1%, v/v). 本研究建立了一個可直接在高含水量且成分複雜之檢品中進行衍生而偵測微量甲醇的高效能液相層析法（HPLC）。以4-[N-methyl, N-（1-naphthylmethyl）]-amino-4-oxobutanoic acid （NAOB）, 4-dimethylaminopyridine （DMAP）和1-ethyl-3-（3-dimethylaminopropyl） carbodiimide hydrochloride （EDC）在溫和的條件下，將水溶液檢品之甲醇順利地進行衍生反應。反應液衍生後可用鹼洗、酸洗來移除有機層中過量的試劑及其他可被酸鹼移除之干擾物質。並對影響衍生反應之諸多因素皆詳加探討，找出最適當的衍生條件。應用此法於五種市售藥酒（乙醇含量8～55%，v／v）中甲醇含量之檢測，其結果為2 .20 × 10-4～3.28 × 10-3% （v／v），皆合乎甲醇含量之衛生標準（<0.1%，v／v）。