国际中医中药杂志
國際中醫中藥雜誌
국제중의중약잡지
International Journal of Traditional Chinese Medicine
2015年
9期
822-825
,共4页
邓雪华%吴红菱%陆连英%李志浩%陈钊宇
鄧雪華%吳紅蔆%陸連英%李誌浩%陳釗宇
산설화%오홍릉%륙련영%리지호%진쇠우
马兜铃酸%排石颗粒%限量测定%固相萃取法
馬兜鈴痠%排石顆粒%限量測定%固相萃取法
마두령산%배석과립%한량측정%고상췌취법
Aristolochic acid%Paishi granule%Limitation%Solid phase extraction
目的 建立排石颗粒中马兜铃酸A的限量检测方法.方法 样品经固相萃取小柱进行处理,采用高效液相色谱法,色谱柱为Phenomenex Luna C18柱(4.6 mm×250 mm,5μm),以乙腈-0.2%碳酸铵溶液(稀盐酸调节pH值为7.5)为流动相,采用梯度洗脱,流速1.0 ml/min,柱温35℃,检测波长250 nm.结果马兜铃酸A在0.029~0.580μg/ml浓度范围内有良好线性关系(r=0.999 9),检测限(S/N=3)为0.9 ng/ml,定量限(S/N=10)为3.0 ng/ml,平均加样回收率为96.4%.结论本方法灵敏度高、准确、重复性好、专属性强,可用于排石颗粒中马兜铃酸A的限量测定.
目的 建立排石顆粒中馬兜鈴痠A的限量檢測方法.方法 樣品經固相萃取小柱進行處理,採用高效液相色譜法,色譜柱為Phenomenex Luna C18柱(4.6 mm×250 mm,5μm),以乙腈-0.2%碳痠銨溶液(稀鹽痠調節pH值為7.5)為流動相,採用梯度洗脫,流速1.0 ml/min,柱溫35℃,檢測波長250 nm.結果馬兜鈴痠A在0.029~0.580μg/ml濃度範圍內有良好線性關繫(r=0.999 9),檢測限(S/N=3)為0.9 ng/ml,定量限(S/N=10)為3.0 ng/ml,平均加樣迴收率為96.4%.結論本方法靈敏度高、準確、重複性好、專屬性彊,可用于排石顆粒中馬兜鈴痠A的限量測定.
목적 건립배석과립중마두령산A적한량검측방법.방법 양품경고상췌취소주진행처리,채용고효액상색보법,색보주위Phenomenex Luna C18주(4.6 mm×250 mm,5μm),이을정-0.2%탄산안용액(희염산조절pH치위7.5)위류동상,채용제도세탈,류속1.0 ml/min,주온35℃,검측파장250 nm.결과마두령산A재0.029~0.580μg/ml농도범위내유량호선성관계(r=0.999 9),검측한(S/N=3)위0.9 ng/ml,정량한(S/N=10)위3.0 ng/ml,평균가양회수솔위96.4%.결론본방법령민도고、준학、중복성호、전속성강,가용우배석과립중마두령산A적한량측정.
Objective To establish a method for the determination of aristolochic acid A inPaishi granule.Methods The HPLC system consisted of the Phenomenex Luna C18(4.6 mm×250 mm, 5μm)column, the mobile phase consisted of acetonitrile and 0.01% HAc, gradient elution flow rate was 1.0 ml/min, the column temperature was 35℃, The UV detector was set at 250 nm.Results The linear response range was 0.029-0.580μg/ml (r=0.999 9). The detection limit and quantitation limit of aristolochic acid A inPaishi granule were 0.9 and 3.0 ng/ml. The average recovery of aristolochic acid A was 96.4%.Conclusion The method is high sensitivity, accurate, repeatable and high specificity,and can be used as an inspection method for safe use of Paishi granule.
