中国药事
中國藥事
중국약사
Chinese Pharmaceutical Affairs
2015年
10期
1069-1073
,共5页
跌打丸%808猩红%高效液相色谱法%液相-质谱联用
跌打汍%808猩紅%高效液相色譜法%液相-質譜聯用
질타환%808성홍%고효액상색보법%액상-질보련용
Dieda Pills%808 Scarlet%HPLC%LC-MS
目的:建立跌打丸中非法染色剂808猩红的检测方法。方法:采用高效液相色谱法,色谱柱为Agilent Eclipse Plus C18柱,柱温30℃,体积流量1.0 mL·min-1,流动相为乙腈-0.02 mol·L-1醋酸铵溶液,梯度洗脱,检测波长516 nm。液质联用验证采用Waters Acquity UPLC BEH C18柱,流动相为乙腈-5 mmol·L-1醋酸铵溶液,梯度洗脱,ESI+扫描模式。供试样品中相关分子离子峰及碎片特征与808猩红对照试剂一致。结果:含量测定808猩红在0.01136~0.11360μg范围内呈良好的线性关系。平均加样回收率为96.95%,RSD为1.14%。结论:该方法简便、快速、准确,专属性、稳定性、重复性良好。
目的:建立跌打汍中非法染色劑808猩紅的檢測方法。方法:採用高效液相色譜法,色譜柱為Agilent Eclipse Plus C18柱,柱溫30℃,體積流量1.0 mL·min-1,流動相為乙腈-0.02 mol·L-1醋痠銨溶液,梯度洗脫,檢測波長516 nm。液質聯用驗證採用Waters Acquity UPLC BEH C18柱,流動相為乙腈-5 mmol·L-1醋痠銨溶液,梯度洗脫,ESI+掃描模式。供試樣品中相關分子離子峰及碎片特徵與808猩紅對照試劑一緻。結果:含量測定808猩紅在0.01136~0.11360μg範圍內呈良好的線性關繫。平均加樣迴收率為96.95%,RSD為1.14%。結論:該方法簡便、快速、準確,專屬性、穩定性、重複性良好。
목적:건립질타환중비법염색제808성홍적검측방법。방법:채용고효액상색보법,색보주위Agilent Eclipse Plus C18주,주온30℃,체적류량1.0 mL·min-1,류동상위을정-0.02 mol·L-1작산안용액,제도세탈,검측파장516 nm。액질련용험증채용Waters Acquity UPLC BEH C18주,류동상위을정-5 mmol·L-1작산안용액,제도세탈,ESI+소묘모식。공시양품중상관분자리자봉급쇄편특정여808성홍대조시제일치。결과:함량측정808성홍재0.01136~0.11360μg범위내정량호적선성관계。평균가양회수솔위96.95%,RSD위1.14%。결론:해방법간편、쾌속、준학,전속성、은정성、중복성량호。
Objective: To establish a method for the detection of illegally added 808 Scarlet in Dieda Pills. Methods:Applying the method of HPLC to an Agilent Eclipse Plus C18 column, 808 Scarlet was separated by using acetonitrile-0.02 mol·L-1 ammonium acetate as the mobile phase under gradient elution. The UV detector was set at 516 nm; the column temperature was at 30℃ and the lfow rate was 1.0 mL·min-1. The method of LC-MS was conducted on a Waters Acquity UPLC BEH C18 column; the mobile phase was composed of acetonitrile and 5 mmol·L-1 ammonium acetate under gradient elution in the ESI+ scanning mode. The ion peaks of related molecules in test samples and fragment features were identical to the reference reagent of 808 Scarlet.Results:808 Scarlet showed good linearity within 0.01136-0.11360 μg and the average recovery was 96.95% (RSD=1.14%). Conclusion:The method is simple, rapid and accurate with good speciifcity, stability and repeatability.