中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2014年
11期
43-48
,共6页
周红霞%杜丹丹%王颖%李慧素%吴宁鹏
週紅霞%杜丹丹%王穎%李慧素%吳寧鵬
주홍하%두단단%왕영%리혜소%오저붕
甲氧苄啶%峰纯度检查%光谱相似度检查%高效液相色谱-二极管阵列检测
甲氧芐啶%峰純度檢查%光譜相似度檢查%高效液相色譜-二極管陣列檢測
갑양변정%봉순도검사%광보상사도검사%고효액상색보-이겁관진렬검측
trimethoprim%peak purity test%spectrum similar test%HPLC-PDA
采用十八烷基键合硅胶为填充剂,以0.02 mol/L磷酸二氢钾溶液-甲醇(73∶27,V/V)为流动相,建立了测定12种兽药中非法添加甲氧苄啶的HP LC-P DA法,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相条件下,对7种兽药粉散剂和5种注射液药物,进行添加回收试验和检测限的测定。结果显示,甲氧苄啶在粉剂中三个浓度(1%、5%、10%)添加回收率为74.6%~115.0%,RSD为0.1%~7.6%,在注射液中三个浓度(0.5%、1%、2%)的添加回收率为87.0%~119.7%,RSD为0.9%~4.1%。甲氧苄啶在各制剂中的检测限为0.5 mg/g(0.25 mg/mL)。改变试验条件后对峰纯度指示、光谱相似度进行考察,仍能满足要求。
採用十八烷基鍵閤硅膠為填充劑,以0.02 mol/L燐痠二氫鉀溶液-甲醇(73∶27,V/V)為流動相,建立瞭測定12種獸藥中非法添加甲氧芐啶的HP LC-P DA法,併採用峰純度檢查和光譜相似度檢查輔助對照品比對方法,對非法添加藥物進行確證。在此液相條件下,對7種獸藥粉散劑和5種註射液藥物,進行添加迴收試驗和檢測限的測定。結果顯示,甲氧芐啶在粉劑中三箇濃度(1%、5%、10%)添加迴收率為74.6%~115.0%,RSD為0.1%~7.6%,在註射液中三箇濃度(0.5%、1%、2%)的添加迴收率為87.0%~119.7%,RSD為0.9%~4.1%。甲氧芐啶在各製劑中的檢測限為0.5 mg/g(0.25 mg/mL)。改變試驗條件後對峰純度指示、光譜相似度進行攷察,仍能滿足要求。
채용십팔완기건합규효위전충제,이0.02 mol/L린산이경갑용액-갑순(73∶27,V/V)위류동상,건립료측정12충수약중비법첨가갑양변정적HP LC-P DA법,병채용봉순도검사화광보상사도검사보조대조품비대방법,대비법첨가약물진행학증。재차액상조건하,대7충수약분산제화5충주사액약물,진행첨가회수시험화검측한적측정。결과현시,갑양변정재분제중삼개농도(1%、5%、10%)첨가회수솔위74.6%~115.0%,RSD위0.1%~7.6%,재주사액중삼개농도(0.5%、1%、2%)적첨가회수솔위87.0%~119.7%,RSD위0.9%~4.1%。갑양변정재각제제중적검측한위0.5 mg/g(0.25 mg/mL)。개변시험조건후대봉순도지시、광보상사도진행고찰,잉능만족요구。
C18 column was used, mobile phase was phosphate buffer and methnol ( 73 ∶ 27, V/V ) , and established a method for determination of trimethoprim in the 12 kinds of veterinary drugs by HPLC-PDA . Peak purity test and spectrum similar test were helped to identify the trimethoprim.Under this liquid condition, the test of added recycling,the determination of detection limit were operated.Results showed that the added recycling rate of TMP in the veterinary powder under three levels ( 1%, 5%, 10%) were 74. 6%~115. 0%, the RSD were 0.1%~7.6%. and injection under three levels (0.5%, 1%, 2%) were 87.0%~119.7%, the RSD were 0.9%~4.1%. Detection limit of trimethoprim in the preparation has got by this method was 0.5 mg/g (0.25 mg/mL). Changing the test conditions,the purity test,spectral similarity can meet the requirements.