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第 47 卷第 3 期Vol. 47 No. 3
2017 年 6 月Jun 2017

所屬欄目:分析與測試

UPLC-MS/MS法同時(shí)檢測大鼠血漿中川陳皮素和紅橘素的濃度
馮 里1,李天雪1,2*,胡玉濤1,2,韋 笑1 (1. 江蘇聯(lián)合職業(yè)技術(shù)學(xué)院 連云港中醫藥分院,江蘇 連云港 222007;2. 連云港市藥物研發(fā)共性技術(shù)中心,江蘇 連云港 222007)
摘 要:建立了同時(shí)測定枳殼中川陳皮素和紅橘素的UPLC-MS方法,并應用于大鼠血漿中的2種化學(xué)成分的濃度監測。色譜柱為Agilent Zorbax Eclipse Plus C18柱(100 mm×2.1 mm,1.8 μm);流動(dòng)相為0.1%甲酸溶液-乙腈;體積流量0.6 mL/min;柱溫30℃;進(jìn)樣量為5 μL;采用電噴霧離子源正離子模式(ESI+),多反應監測進(jìn)行測定(MRM)。結果顯示,川陳皮素和紅橘素分別在1~500 ng/mL和1~750 ng/mL內具有良好的線(xiàn)性關(guān)系(r2≥0.998),兩成分的日內和日間精密度的RSD值均小于7.2%,準確度為95.2%~104.2%,基質(zhì)效應在87.5%~114.6%合理范圍內,平均回收率為85.5%~92.2%。本方法經(jīng)方法學(xué)驗證,可對川陳皮素和紅橘素同時(shí)進(jìn)行血藥濃度檢測,降低了分析成本,為臨床用藥研究提供了有效的分析手段。
關(guān)鍵詞:枳殼;川陳皮素;紅橘素;高效液相色譜質(zhì)譜聯(lián)用
中圖分類(lèi)號:  文獻標識碼:A  文章編號:1009-9212(2017)03-0067-05
Simultaneous Determination of the Nobiletin and Tangeretin in Rat Plasma by UPLC-MS/MS
FENG Li1, LI Tian-xue1,2*, HU Yu-tao1,2, WEI Xiao1 (1. Lianyungang TCM Branch of Jiangsu Union Technical Institute, Lianyungang 222007, China; 2. Lianyungang Common Technological Center for Drug Research and Development, Lianyungang 222007, China)
Abstract:An ultra-high performance liquid chromatographic method was established to simultaneously determine the contains of the nobiletin and tangeretin in Fructus aurantii(ZhiQiao). This method was further applied in the determination of nobiletin and tangeretin in rat plasma after oral administration of ZhiQiao extract. The LC column was Agilent Zorbax Eclipse Plus C18(100 mm×2.1 mm, 1.8 μm). The mobile phase was comprised of acetonitrile and water containing 0.1% formic acid. Flow rate was set at 0.6 mL/min. Column temperature was kept at 30℃. The quantification was obtained by scanning with multiple reaction monitoring (MRM) via the positive electrospray ionization (ESI+) source. The correlation coefficients of the nobiletin and tangeretin were respectively over 0.998 in the ranges of 1~500 ng/mL, 1~750 ng/mL. The RSD values of the inter-and intra-precisions were less than 7.2%. The accuracy ranged from 95.2% to 104.2%. The matrix effect values were sufficiently minimized to 87.5%~114.6%. The average recoveries from rat plasma were 85.5% to 92.2%. This method could significantly reduce the analysis cost, and provide an analytic method for the clinical medication adjustment.
Key words:Fructus aurantii L.; nobiletin; tangeretin; LC-MS/MS
基金項目:連云港市521人才資助項目(2016)。
作者簡(jiǎn)介:馮 里(1982-),男,江蘇連云港人,碩士,講師,主要從事藥理學(xué)專(zhuān)業(yè)研究(E-mail:907773517@qq.com)。
聯(lián) 系 人:李天雪,碩士,講師,主要從事藥物分析研究(E-mail:litx1988@126.com)。
收稿日期:2017-06-04
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