中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2014年
8期
47-50
,共4页
刘雪红%董紫凌%韩凤丽%郑洁%马慧楠%宋平%田晓玲
劉雪紅%董紫凌%韓鳳麗%鄭潔%馬慧楠%宋平%田曉玲
류설홍%동자릉%한봉려%정길%마혜남%송평%전효령
清瘟败毒散%金刚烷胺%超高效液相色谱-串联质谱
清瘟敗毒散%金剛烷胺%超高效液相色譜-串聯質譜
청온패독산%금강완알%초고효액상색보-천련질보
Qingwen Baidu San%amantadine%Ultra-HPLC-MS-MS
应用超高效液相色谱-串联质谱技术,建立了兽用中药制剂清瘟败毒散中非法添加金刚烷胺的检测方法。样品经提取液提取后,稀释。采用0.2%甲酸水溶液与甲醇作为流动相进行梯度洗脱,经BEH C18色谱柱分离,通过多反应监测模式进行测定。金刚烷胺在0.05~25 ng/mL的范围内线性关系良好,相关系数大于0.999;平均回收率为86.9%~95.2%,批内、批间相对标准偏差均小于3.8%,检测限为0.025 mg/g,定量限为0.1 mg/g。该法准确、简单、快速,可用于清瘟败毒散中非法添加金刚烷胺的检测。
應用超高效液相色譜-串聯質譜技術,建立瞭獸用中藥製劑清瘟敗毒散中非法添加金剛烷胺的檢測方法。樣品經提取液提取後,稀釋。採用0.2%甲痠水溶液與甲醇作為流動相進行梯度洗脫,經BEH C18色譜柱分離,通過多反應鑑測模式進行測定。金剛烷胺在0.05~25 ng/mL的範圍內線性關繫良好,相關繫數大于0.999;平均迴收率為86.9%~95.2%,批內、批間相對標準偏差均小于3.8%,檢測限為0.025 mg/g,定量限為0.1 mg/g。該法準確、簡單、快速,可用于清瘟敗毒散中非法添加金剛烷胺的檢測。
응용초고효액상색보-천련질보기술,건립료수용중약제제청온패독산중비법첨가금강완알적검측방법。양품경제취액제취후,희석。채용0.2%갑산수용액여갑순작위류동상진행제도세탈,경BEH C18색보주분리,통과다반응감측모식진행측정。금강완알재0.05~25 ng/mL적범위내선성관계량호,상관계수대우0.999;평균회수솔위86.9%~95.2%,비내、비간상대표준편차균소우3.8%,검측한위0.025 mg/g,정량한위0.1 mg/g。해법준학、간단、쾌속,가용우청온패독산중비법첨가금강완알적검측。
A method of Ultra-HPLC-MS/MS was developed to determine amantadine illegally added in Qingwen Baidu San of traditional chinese medicine for animals. The samples were extracted and diluted. The HPLC separation was performed on BEH C18 column with a linear gradient elution program of methanol and 0.2% formic acid solution as the mobile phase. Selective reaction monitoring was used for the selective detection .The linearity of amantadine ranged 0.05 to 25 ng/mL with coefficient greater than 0.999. The average recorvery was 86.9%~95.2%and RSD of intra-batch and inter-batch were both less than 3. 8%. The limit of detection was 0. 025 mg/g and limit of quantification was 0. 1 mg/g. The method was accurate, convenient, fast and can be used as a determination for illegally added amamtadine in Qingwen Baidu San.