中国药学(英文版)
中國藥學(英文版)
중국약학(영문판)
JOURNAL OF CHINESE PHARMACEUTICAL SCIENCES
2005年
1期
38-42
,共5页
李妮%黄建明%翁伟宇%黄照昌%蔡佳%郁韵秋
李妮%黃建明%翁偉宇%黃照昌%蔡佳%鬱韻鞦
리니%황건명%옹위우%황조창%채가%욱운추
灯盏乙素%液质联用%固相萃取%灯盏花素
燈盞乙素%液質聯用%固相萃取%燈盞花素
등잔을소%액질련용%고상췌취%등잔화소
scutellarin%LC-MS%SPE%breviscapine
目的建立灵敏、专属的HPLC-ESI-MS测定法, 用于测定家兔口服灯盏花素缓释片(2片 60 mg/片)后的血药浓度.方法该定量方法采用芦丁作内标,用固相萃取(SPE)进行样品前处理.以甲醇10 mmol·L-1醋酸铵水溶液(pH 8.0)梯度洗脱,流动相流速0.4 mL·min-1,柱温35 ℃,经过Zorbax Extend-C18 (150 mm×2.1 mm ID, 5 μm)色谱柱分离,电喷雾质谱检测器在负离子模式下检测灯盏乙素和芦丁.结果在2~200 ng·mL-1范围内灯盏乙素与内标峰面积与浓度线性关系良好,且准确度、精密度满足生物样品分析的要求.结论本实验建立的兔血浆中灯盏乙素的HPLC-MS分析方法灵敏度高,可用于口服给药后灯盏乙素的血药浓度测定.
目的建立靈敏、專屬的HPLC-ESI-MS測定法, 用于測定傢兔口服燈盞花素緩釋片(2片 60 mg/片)後的血藥濃度.方法該定量方法採用蘆丁作內標,用固相萃取(SPE)進行樣品前處理.以甲醇10 mmol·L-1醋痠銨水溶液(pH 8.0)梯度洗脫,流動相流速0.4 mL·min-1,柱溫35 ℃,經過Zorbax Extend-C18 (150 mm×2.1 mm ID, 5 μm)色譜柱分離,電噴霧質譜檢測器在負離子模式下檢測燈盞乙素和蘆丁.結果在2~200 ng·mL-1範圍內燈盞乙素與內標峰麵積與濃度線性關繫良好,且準確度、精密度滿足生物樣品分析的要求.結論本實驗建立的兔血漿中燈盞乙素的HPLC-MS分析方法靈敏度高,可用于口服給藥後燈盞乙素的血藥濃度測定.
목적건립령민、전속적HPLC-ESI-MS측정법, 용우측정가토구복등잔화소완석편(2편 60 mg/편)후적혈약농도.방법해정량방법채용호정작내표,용고상췌취(SPE)진행양품전처리.이갑순10 mmol·L-1작산안수용액(pH 8.0)제도세탈,류동상류속0.4 mL·min-1,주온35 ℃,경과Zorbax Extend-C18 (150 mm×2.1 mm ID, 5 μm)색보주분리,전분무질보검측기재부리자모식하검측등잔을소화호정.결과재2~200 ng·mL-1범위내등잔을소여내표봉면적여농도선성관계량호,차준학도、정밀도만족생물양품분석적요구.결론본실험건립적토혈장중등잔을소적HPLC-MS분석방법령민도고,가용우구복급약후등잔을소적혈약농도측정.
Aim To establish a sensitive and specific liquid chromatography-mass spectrometry method for determination of scutellarin in rabbit plasma after oral administration. Methods For the quantitative analysis, rutin was used as an internal standard and solid-phase extraction (SPE) was performed by using a Phenomenex C8 cartridge. HPLC was carried out using a Zorbax Extend-C18column (150 mm×2.1 mm ID, 5 μm) with a guard cartridge (Phenomenex). Gradient elution was selected with the mobile phase of methanol 10 mmol·L-1 ammonium acetate solution (pH adjusted to 8.0 with ammonia solution). The flow rate of mobile phase was 0.4 mL·min-1 and the column temperature was 35 ℃. Both scutellarin and the internal standard rutin in rabbit plasma extracts were detected by mass spectrometry using an ESI interface in the negative ion mode. Results The linear range was from 2 to 200 ng·mL-1, with acceptable accuracy and precision (RSD). Conclusion A sensitive, reliable and accurate method for the quantitation of scutellarin in rabbit plasma has been established.