趙俊杰 錢一鑫 康冀川 何珺
摘要:以左旋龍腦標準品為對照,應用高效液相色譜法(High Performance Liquid Chromatography HPLC)(條件:Neptune C-18色譜柱,甲醇-04%磷酸(65∶35)為流動相,流速08mL/min,柱溫25℃)對咽炎清片中左旋龍腦的含量進行測定,結(jié)果發(fā)現(xiàn)左旋龍腦在10~100μg/mL范圍內(nèi)呈現(xiàn)良好的線性關系,其回歸方程為Y=13687X-21173(r=09997,n=6),加樣回收率為1033%,RSD為042%,同時該方法操作簡便,分析快速,方法學考察結(jié)果符合有關新藥研究的技術要求及《中國藥典》2015年版第四部通則中對于高效液相色譜法的各項規(guī)定,適宜用于咽炎清片中左旋龍腦含量測定。
關鍵詞:示差檢測器;咽炎清;左旋龍腦;高效液相色譜
中圖分類號:R917;O6577
文獻標識碼:A
文章編號:1008-0457(2017)02-0074-04國際DOI編碼:10.15958/j.cnki.sdnyswxb.2017.02.016
Abstract:The concentration of L-borneol in Yanyanqing Tablet was determined by High Performance Liquid Chromatography (HPLC) (Conditions: C-18 Neptune column, methanol -04% phosphoric acid (65∶35) as the mobile phase, flow rate 08mL/min, column temperature 25℃). The results showed that the concentration of L-borneol had a good linear relationship within the range of 10-100μg/mL. The regression equation was Y=13687X-21173 (r=09997, n=6). The average recovery was 1033%, while RSD was 042%. It is an easy and fast approach that meet the requirements for developing new drug, as well as Chinese Pharmacopoeia 2015 (the fourth volume), by methodological study. The method is suitable for determining the concentration of L-borneol in Yanyanqing Tablet.
Key words:refractive index detector; Yanyanqing tablet; L-borneol; HPLC
示差檢測器(Refractive index detector, RID)是目前HPLC法中常用的一種檢測器,它可與輸液泵、色譜柱、進樣器等組成凝膠滲透色譜儀或高速液相色譜儀系統(tǒng),也可以配置適當?shù)倪M樣系統(tǒng)作為單獨的分析儀器使用,同時對所有溶質(zhì)都有響應。某些不能用選擇性檢測器檢測的組分,可用示差檢測器檢測。由于不同的液體折光不同,因此該檢測器通用性強,可廣泛地應用于化工、石油、醫(yī)藥、食品等領域。示差檢測器是基于連續(xù)測定樣品流路和參比流路之間折射率的變化來測定樣品含量的。光從一種介質(zhì)進入另一種介質(zhì)時,由于兩種物質(zhì)的折射率不同就會產(chǎn)生折射。只要樣品組分與流動相的折光指數(shù)不同,就可被檢測,二者相差愈大,靈敏度愈高,在一定濃度范圍內(nèi)檢測器的輸出與溶質(zhì)濃度成正比[1]。
咽炎清片為貴州苗族藥驗方,是由腫節(jié)風、左旋龍腦和薄荷腦3味組成,味甜,微澀;……