以矽膠管柱搭配含水移動相之高壓液相層析法同時定量陽離子殺菌劑成分   全文下載

Simultaneous Quantitation of Cationic Disinfectants by High-Performance Liquid Chromatography on a Silica Gel Column Using Aqueous Eluents

本研究已發展出一種簡單、快速及正確之高壓液相層析法以矽膠管柱搭配含水移動相用以定量陽離子殺菌劑成分。首先將這些殺菌劑區分為兩類，使用μ-Porasil矽膠管柱（3.9公釐內徑×300公釐）皆可同時分離所添加之殺菌劑。使用第一種含水移動相，其組成為乙?：水（70／30，v／v），0.04% 三乙基胺及0.1% 醋酸，紫外光檢測波長設定為262 nm，可定量添加於化妝品中之氯化莘二甲煙銨（1）及葡萄糖酸洛赫西定（2），以氫溴酸右旋美索芬為內在標準品，可於九分鐘內偵測出每一種化妝品檢品中所含之上列兩種陽離子殺菌劑。第二種含水移動相之組成為乙?：水（90／10，v／v），0.04% 三乙基胺及0.1% 醋酸，紫外光檢測波長為269 nm，可同時定量添加於藥品中之溴化多米芬（3）、氯化本索寧（4）、氯化鯨蠟?啶（5）及氯化氯狹那（6）。以溴化普泮夕林為內在標準品，可於16分鐘內定量每一種藥物檢品中所含之上列四種陽離子殺菌劑。此分析法提供一種可靠及快速的方式以分析日常家用之化妝品及藥品中陽離子殺菌劑成分。由六種陽離子殺菌劑標準品所得之六條標準直線之線性回歸顯示相關係數，r2，介於0.9997~ 1.0000之間。本高壓液相層析法具有高標準之精密度及準確度，由日內及日間誤差分析結果：化妝品檢品之變異係數介於0.13~2.04%之間；藥物檢品之變異係數則介於0.08~0.87%。化妝品檢品之回收率為96.75~99.75%，變異係數為0.45~2.88%；藥物檢品之回收率為99.17~99.92%，變異係數為0.21~0.47%。

A simple, rapid, and accurate high-performance liquid chromatographic (HPLC) method for quantitation of cationic disinfectants was developed using a silica gel column with aqueous mobile phases. The disinfectants are classified into two categories, both of which can be separated simultaneously on a μ-Porasil silica gel column (3.9 × 300 mm). An aqueous mobile phase (1), composed of CH3CN: H2O (70/30, v/v), triethylamine (0.04%), and acetic acid (0.1%), with UV detection at 262 nm, provides quantitation of benzalkonium chloride (1) and chlorhexidine gluconate (2) in cosmetics. The identification of two cationic disinfectants in each cosmetic sample can be achieved in 9 min with dextromethorphan HBr as an internal standard. With the mobile phase (2) of CH3CN: H2O (90/10, v/v), triethylamine (0.04%), and acetic acid (0.1%), setting the UV detection at 269 nm can identify the constituents of domiphen bromide (3), benzethonium chloride (4), cetylpyridium chloride (5), and dequalinium chloride (6) in pharmaceuticals. When propantheline bromide was used as an internal standard, the quantitation of four cationic disinfectants in each pharmaceutical sample could be completed within 16 min. The method provides a reliable, prompt way to analyze cationic disinfectants in both household cosmetics and pharmaceutical preparations available on the market. Regression equations of six standard curves revealed the related coefficients, r2, of between 0.9997 and 1.0000. The HPLC method can be carried out with a high level of precision and accuracy. From the intra- and interday tests, the coefficients of variation (CV) were between 0.13% and 2.04% for cosmetics, and 0.08% and 0.87% for pharmaceuticals. The recoveries were found to be 96.75%~99.95% for cosmetics with CV of 0.45%~2.88%, and 99.17%~99.92% for pharmaceuticals with CV of 0.21%~0.47%. 本研究已發展出一種簡單、快速及正確之高壓液相層析法以矽膠管柱搭配含水移動相用以定量陽離子殺菌劑成分。首先將這些殺菌劑區分為兩類，使用µ-Porasil矽膠管柱（3.9公釐內徑×300公釐）皆可同時分離所添加之殺菌劑。使用第一種含水移動相，其組成為乙腈：水（70／30，v／v），0.04% 三乙基胺及0.1% 醋酸，紫外光檢測波長設定為262 nm，可定量添加於化妝品中之氯化莘二甲煙銨（1）及葡萄糖酸洛赫西定（2），以氫溴酸右旋美索芬為內在標準品，可於九分鐘內偵測出每一種化妝品檢品中所含之上列兩種陽離子殺菌劑。第二種含水移動相之組成為乙腈：水（90／10，v／v），0.04% 三乙基胺及0.1% 醋酸，紫外光檢測波長為269 nm，可同時定量添加於藥品中之溴化多米芬（3）、氯化本索寧（4）、氯化鯨蠟吡啶（5）及氯化氯狹那（6）。以溴化普泮夕林為內在標準品，可於16分鐘內定量每一種藥物檢品中所含之上列四種陽離子殺菌劑。此分析法提供一種可靠及快速的方式以分析日常家用之化妝品及藥品中陽離子殺菌劑成分。由六種陽離子殺菌劑標準品所得之六條標準直線之線性回歸顯示相關係數，r2，介於0.9997～ 1.0000之間。本高壓液相層析法具有高標準之精密度及準確度，由日內及日間誤差分析結果：化妝品檢品之變異係數介於0.13～2.04%之間；藥物檢品之變異係數則介於0.08～0.87%。化妝品檢品之回收率為96.75～99.75%，變異係數為0.45～2.88%；藥物檢品之回收率為99.17～99.92%，變異係數為0.21～0.47%。