HPLC_MS_MS法测定中药材枳壳中展青霉素_王少敏

LC-MS/MS法同时测定大鼠血浆中贝母素甲、贝母素乙的浓度及其在药代动力学中的应用陈丽华1, 刘丽丽2, 刘红宁1, 朱卫丰1*, 衣文娇1, 赵益1 (江西中医学院 1. 现代中药制剂教育部重点实验室, 江西南昌 330004; 2. 科技学院, 江西南昌 330025)摘要: 建立同时测定大鼠灌胃及静注给予浙贝母提取物后血浆中贝母素甲及贝母素乙含量的HPLC-MS/MS 分析方法, 并计算2种生物碱在大鼠体内的药代动力学参数。

血浆样品经乙酸乙酯液-液萃取后, 以乙腈-10 mmol·L−1甲酸铵水溶液 (35∶65) 为流动相, Luna C18色谱柱(150 mm × 2 mm ID, 3 µm) 分离, 采用电喷雾离子化源 (ESI) 三重四极杆串联质谱, 以多反应监测模式 (MRM) 进行检测, 检测离子对分别为m/z 432.4 → 414.4 (贝母素甲)、m/z 430.4 → 412.4 (贝母素乙) 和m/z 237.1 → 194.2 (内标, 卡马西平)。

贝母素甲及贝母素乙均在0.8～800 ng·mL−1内呈良好线性关系, 提取回收率分别为94.1%～105.3%和85.8%～98.6%。

方法的精密度、准确度和稳定性均符合要求。

结果显示, 该法选择性强、灵敏度高、操作简便, 适用于贝母素甲、贝母素乙的大鼠药代动力学研究。

关键词: 贝母素甲; 贝母素乙; 浙贝母提取物; 药代动力学; LC-MS/MS; 血浆中图分类号: R917 文献标识码:A 文章编号: 0513-4870 (2010) 07-0891-04Simultaneous determination of peimine and peiminine in rat plasma by LC-MS/MS and its application in the pharmacokinetic studyCHEN Li-hua1, LIU Li-li2, LIU Hong-ning1, ZHU Wei-feng1*, YI Wen-jiao1, ZHAO Yi1(1. Key Laboratory of Modern Preparation of Traditional Chinese Medicine, Ministry of Education, Jiangxi University of TCM,Nanchang 330004, China; 2. Science and Technology College, Jiangxi University of TCM, Nanchang 330025, China)Abstract: To establish an LC-MS/MS method for simultaneous determination of peimine and peiminine in rat plasma after oral and intravenous administration of Fritillaria thunbergii Miq. extract, the pharmacokinetic parameters were calculated as well. Peimine, peiminine and internal standard carbamazepine were extracted from plasma with liquid-liquid extraction by ethyl acetate, then separated on a Luna C l8 column by using acetonitrile- water containing 10 mmol·L−1 ammonium formate (35∶65), as mobile phase. The electrospray ionization (ESI) source was applied and operated in positive ion mode. Peimine was detected at m/z 432.4 → 414.4, peiminine at m/z 430.4 → 412.4 and carbamazepine (IS) at 237.1 → 194.2. The linear calibration curves were obtained at the concentration range of 0.8 − 800 ng·mL−1 for peimine and peiminine. The extraction recoveries were94.1%−105.3% and 85.8%−98.6%, respectively. The precisions, accuracy and stability of the analytes meet therequirements. The method was shown to be effective, convenient, and suitable for simultaneous pharmacokinetic study of peimine and peiminine in rat.Key words: peimine; peiminine; Fritillaria thunbergii Miq.extract; pharmacokinetics; LC-MS/MS; plasma收稿日期: 2009-12-25.基金项目: 江西省自然科学基金资助项目 (2008GZY0115); 江西省教育厅项目 (GJJ09544).*通讯作者 Tel: 86-791-7119011, Fax: 86-791-7118658, E-mail: zwflady@浙贝母为百合科植物浙贝母(Fritillaria thunbergii Miq.)的干燥鳞茎, 具有止咳祛痰、镇痛抗炎等功效[1]。

陈皮青皮和枳壳中黄酮类成分的指纹图谱研究进展
邵红霞;代云桃;秦雪梅;张丽增
【期刊名称】《山西医药杂志》
【年(卷),期】2007(036)019
【总页数】3页(P898-900)
【作者】邵红霞;代云桃;秦雪梅;张丽增
【作者单位】山西大学化学化工学院,030006;山西大学化学化工学院,030006;山西大学化学化工学院,030006;山西大学化学化工学院,030006
【正文语种】中文
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1.青皮不同炮制品中黄酮类成分的试验比较 [J], 郑青山
2.不同产地枳实与枳壳中黄酮类成分的含量测定 [J], 王青;袁丹
3.SPE-HPLC-DAD法同时检测柑橘药用资源中黄烷酮类和川陈皮素成分 [J], 谢辉; 陈亚; 雷爱玲; 朱春燕; 李杨梅; 白玉婷; 孙鹏; 李贵节
4.不同年份陈皮指纹图谱及黄酮类成分含量测定 [J], 周洁;黄海龙;余虹;高慧;李晶;叶喜德
5.不同方法提取陈皮中黄酮类有效成分含量比较 [J], 张婷婷;梁燕;彭灿
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枳壳药材挥发油的GC—MS指纹图谱研究目的：建立枳壳药材挥发油的气相色谱-质谱（GC-MS）指纹图谱。

方法：采用GC-MS法，色谱柱为RTX-5MS毛细管柱，进样口温度为250 ℃，载气为高纯氦气（≥99.999%），流速为1.0 mL/min，分流比为10 ∶1，进样量为1 μL （程序升温）；采用电子轰击离子源，离子源温度为230 ℃，检测器温度为250 ℃，溶剂延迟时间为3 min，扫描范围为m/z 35～550。

以月桂烯为参照，测定21批药材挥发油样品的GC-MS图谱，采用《中药色谱指纹图谱相似度评价系统》（2004 A版）进行相似度评价，确定共有峰，采用LC Solution 2质谱库（NIST05.LIB和NIST05s.LIB）确定共有峰成分，并采用面积归一化法测定共有峰的相对含量。

结果：21批药材挥发油样品的GC-MS图谱有20个共有峰，相似度均>0.90；经验证，21批药材挥发油样品GC-MS图谱与对照指纹图谱具有较好的一致性。

枳壳药材挥发油主要成分为柠檬烯、萜品烯、月桂烯和D-Cadinene。

结论：所建指纹图谱可为枳壳药材挥发油的真伪鉴别和质量评价提供参考。

ABSTRACT OBJECTIVE：To establish GC-MS fingerprint of volatile oil from Citrus aurantium. METHODS：GC-MS method was adopted. The determination was performed on RTX-5MS capillary column with injector temperature of 250 ℃，high pure helium as carrier gas（≥99.999%），flow rate of 1.0 mL/min，split ratio of 10 ∶1，and sample size of 1 μL （temperature programming）. Mass spectrum condition included electron bombardment ion source，ion source temperature of 230 ℃，detector temperature of 250 ℃，3 min solvent delay，scanning range of m/z 35-550. GC-MS chromatograms of 21 batches of volatile oil samples were determined using Laurene as reference. The similarity of them was evaluated by using TCM Chromatographic Fingerprint Similarity Evaluation System （2004 A edition），and common peak was determined. The components of common peak were determined by LC Solution 2 mass database （NIST05.LIB and NIST05s.LIB）. Relative content of common peak was determined with area normalization. RESULTS：There were 20 common peaks in GC-MS chromatograms of 21 batches of volatile oil samples，and the similarity was higher than 0.90. After validation，GC-MS chromatograms of 21 batches of volatile oil samples were in good agreement with control fingerprint. The main constituents of the volatile oil of C. aurantium were Limonene，Terpinene，Laurene and D-Cadinene. CONCLUSIONS：Established fingerprint can provide reference for identification and quality evaluation of volatile oil of C. aurantium.KEYWORDS Citrus aurantium；V olatile oil；GC-MS fingerprint；Genuine regional drug枳殼为芸香科植物酸橙（Citrus aurantium L.）及其栽培变种的干燥未成熟果实[1]，有理气宽中之功效，多用于食积不化、脘腹胀满等症状[2]。

HPLC-ESI-MS／MS快速测定泽兰水提物中的7种成分强光辉;刘昆善;姚宏武;李军【期刊名称】《西北药学杂志》【年(卷),期】2015(30)6【摘要】目的：建立泽兰水提物中主要成分咖啡酸、迷迭香酸、熊果酸、芦丁、木犀草素、齐墩果酸和槲皮素快速测定的超高效液相色谱‐电喷雾‐三重四级杆串联质谱方法。

方法超声法制备泽兰水提物，XBridge‐C18（100 mm ×2．1 mm ，3．5μm）反相梯度洗脱法对样品进行分离；电喷雾电离源负离子模式多级反应监测扫描法对各成分进行定量分析。

结果方法的相对标准偏差在0．24％～2．8％范围内，回收率在93．3％～105．2％之间，检测限为0．05～1．0μg · L －1。

结论该方法具有分析速度快，灵敏度高和特异性强的特点，可为中药中目标成分的含量测定提供方法学参考。

%Objective To develop a method for rapid and simultaneous determination of rosmarinci acid ,caffeic acid ,ursolicacid ,cya‐nidenon ,phytomelin ,oleanolic acid and quercetin by ultra‐performance liquid chromatography‐electrospray‐triple quadrupole mass spectrometer .Methods Ultrasonic method was used to prepare the aqueous extract of Lycopus lucidus Turcz .;an XBridge‐C18re‐verse phase column was employed to separate the interest compounds through gradient elution ;multi reaction monitoring method under electrospray ionization and negative ion mode was utilized to determine the seven compounds .Results The relative standard deviations of the method werein the range of 0 .24%‐2 .8% ;the recoveries were ranged from 93 .3%‐105 .2% ;the limits of detec‐tion were 0 .05‐1 .0 μg · L -1 .Conclusion The proposed method has the advantages of rapid speed of analysis ,high sensitivity and specificity .It is possible to become an alternative for the determination of target compounds in traditional Chinese medicine .【总页数】4页(P693-696)【作者】强光辉;刘昆善;姚宏武;李军【作者单位】西安市自来水有限公司，西安 710082;西安市自来水有限公司，西安 710082;西安市自来水有限公司，西安 710082;西安市自来水有限公司，西安710082【正文语种】中文【中图分类】R282【相关文献】1.HPLC-ESI-MS/MS快速测定鱼肉中的氯霉素残留 [J], 李资玲;黄优生;熊向源;李玉萍;吴光杰2.LC-MS/MS法同时测定犬血浆中7种人参皂苷类成分及其在人参提取物药代动力学研究中的应用 [J], 林力;刘建勋;张颖;李欣志;段昌令;林成仁;李磊3.HPLC-ESI-MS法同时测定印度獐牙菜中5种酮类化合物的含量 [J], 张大业;陈丽娟;刘健4.UPLC-MS/MS法快速测定龟甲胶中龟源成分 [J], 郭尚伟;庞慧慧;段小波;徐云鹏;王玉娇;赵婷婷;黄雅钦5.HPLC-ESI-MS/MS法同时测定血必净注射液中11种有效成分的含量 [J], 王红;刘玲;苏联麟;郭志花;崔永伟因版权原因，仅展示原文概要，查看原文内容请购买。

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