UPLC-MS/MS测定beagle犬内西罗莫司血药浓度

陈咏; 林晨; 张晶; 邱彬; 周欣; 宋洪涛

留言板

尊敬的读者、作者、审稿人, 关于本刊的投稿、审稿、编辑和出版的任何问题, 您可以本页添加留言。我们将尽快给您答复。谢谢您的支持!

姓名
邮箱
手机号码
标题
留言内容
验证码

x 关闭永久关闭

重要提示

《药学实践与服务》杂志不接收生物战剂、毒剂相关内容的稿件。对于涉军信息类论文如需投稿，请务必投稿前电话或邮箱咨询。联系电话：021-81871323，邮箱：yxsjzzs@163.com。敬请谅解，谢谢配合！

《药学实践与服务》编辑部

免责声明

《药学实践与服务》杂志目前不收取审稿费、版面费、加急费等费用，如收到邮件声称是编辑部X编辑，要求加作者微信的，请谨防财产损失！编辑部用于作者校稿时微信绑定的邮件是通过yxsjzzs@163.com发送的，标题是《药学实践与服务》XML数字出版服务微信绑定，请区分开！

UPLC-MS/MS测定beagle犬内西罗莫司血药浓度

陈咏, 林晨, 张晶, 邱彬, 周欣, 宋洪涛

文章导航 > 药学实践与服务 > 2011 > 29(5): 353-355,375

陈咏, 林晨, 张晶, 邱彬, 周欣, 宋洪涛. UPLC-MS/MS测定beagle犬内西罗莫司血药浓度[J]. 药学实践与服务, 2011, 29(5): 353-355,375.

引用本文:

陈咏, 林晨, 张晶, 邱彬, 周欣, 宋洪涛. UPLC-MS/MS测定beagle犬内西罗莫司血药浓度[J]. 药学实践与服务, 2011, 29(5): 353-355,375.

CHEN Yong, LIN Chen, ZHANG Jing, QIU Bin, ZHOU Xin, SONG Hong-tao. Determination of sirolimus in whole blood of beagle dog by UPLC-MS/MS[J]. Journal of Pharmaceutical Practice and Service, 2011, 29(5): 353-355,375.

Citation:

CHEN Yong, LIN Chen, ZHANG Jing, QIU Bin, ZHOU Xin, SONG Hong-tao. Determination of sirolimus in whole blood of beagle dog by UPLC-MS/MS[J]. Journal of Pharmaceutical Practice and Service, 2011, 29(5): 353-355,375.

UPLC-MS/MS测定beagle犬内西罗莫司血药浓度

陈咏¹,
林晨²,
张晶³,
邱彬⁴,
周欣³,
宋洪涛^3,

1.
福州大学化学化工学院 ,福建福州 350002;福建卫生职业技术学院,福建福州 350101
2.
福建省药品检验所,福建福州 350025
3.
南京军区福州总医院药学科,福建福州 350025
4.
福州大学化学化工学院 ,福建福州 350002

Determination of sirolimus in whole blood of beagle dog by UPLC-MS/MS

1.
Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China;Fujian Medical College, Fuzhou 350101, China
2.
Fujian institute for Drug Control, Fuzhou 350025, China
3.
Deptment of Pharmacy, Fuzhou General Hospital of Nanjing Military Command, Fuzhou 350025, China
4.
Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China

摘要: 目的建立测定beagle犬内西罗莫司(SRL)血药浓度的UPLC-MS/MS联用方法。方法色谱柱为Agilent C₁₈柱(50 mm × 2.1 mm,1.7 μm,);预柱为C₁₈柱(4.0 mm × 3.0 mm,5 μm);流动相为乙腈-水(90:10,v/v);流速为 0.30 ml/min;柱温为50℃;进样室温度为4 ℃。离子源为ESI源;正离子方式检测;扫描方式为多反应监测(MRM);用于定量分析的离子反应分别为m/z 936.6→m/z 409.7(西罗莫司)和m/z 826.6→m/z 415.4(内标他克莫司)。取全血样品经液-液萃取后进样20 μl。结果 SRL在0.50~12.00 ng/ml浓度范围内呈良好的线性(r=0.999 7),定量下限0.5 ng/ml,日内、日间精密度(RSD)均小于15%,方法回收率均大于90%,萃取回收率大于76%。结论本方法具有样品处理简单,方法灵敏、快速、选择性强,满足西罗莫司在beagle犬体内药物检测的要求。
- 西罗莫司 /
- 超高效液相色谱-质谱联用 /
- 血药浓度
Abstract: Objective To develop a UPLC-MS/MS method for the determination of sirolimus in whole blood of beagle dog. Methods Sirolimus and internal standard Tacrolimus were extracted from whole blood with liquid-liquid extraction,then separated on a Agilent C₁₈ column (50 mm ×2.1 mm,1.7 μm) at the flow-rate of 0.30 ml/min. The mobile phase was Acetonitrile-water (90∶10) and the column temperature was 50 ℃. Electrospray ionization ( ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 936.6→409.7 and m/z 826.6→415.4 were used to quantify sirolimus and the internal standard,respectively. Results The calibration linea range of blood-Sirolimu concentrations was 0.50~12.00 ng/ml(r=0.999 7).The low limit of quantification was 0.50 ng/ml . The intra-and inter-day precisions (RSDs) were less than 15%. The method recoveries were more than 90% . The extraction recoveries were more than 76%. Conclusions The method was specific,sensitive,rapid and suitable for the pharmacokinetic study of sirolimus in whole blood of beagle dog.
- sirolimus /
- UPLC-MS/MS /
- whole blood

[1]	朱曼,郭代红.新型大环内酯类免疫制剂——西罗莫司[J].中国药物应用与监测,2005(6):26.
[2]	Yáñez JA,Forrest ML,Ohgami Y,et al. Pharmacometrics and delivery of novel nanoformulated PEG-b-poly (ε-cap-rolactone) micelles of rapamycin[J]. Cancer Chemoth Pharm,2008,61(1) : 133.
[3]	Ren B,Li SX,Deng B, et al. Determination of sirolimus in human whole blood by HPLC[J]. Chin Pham J,2004,39(1):52.
[4]	Lee JH,Cha KH,Cho W,et al. Quantitative determination of sirolimus in dog blood using liquid chromatography-tandem mass spectrometry, and its applications to pharmacokinetic studies[J].Journal of Pharmaceutical and Biomedical Analysis,2010,53(4):1042 .
[5]	张东娣,范艳花.液-质联用在西罗莫司和依维莫司血药浓度监测中的应用进展[J].商丘师范学院学报,2007,23(12):90.
[6]	时颖华,李中东,施孝金,等. HPLC法测定人全血中西罗莫司的浓度[J].中国临床药学杂志,2O04,13(2):76.
[7]	孙明辉,斯陆勤,翟雪珍,等.高效液相色谱-质谱联用测定大鼠体内西罗莫司血药浓度[J]. 中国药学杂志,2O10,45(2):132.
[8]	祝仕清,牛长群. UPLC(超高效液相色谱)/MS/MS联用技术测定全血中的西罗莫司[J]. 中国抗生素杂志,2007,32(6):347.
[9]	董振南,贾兴旺,王玲,等. 微粒子酶联免疫吸附法测定西罗莫司血药浓度的方法学评价[J].军医进修学院学报,2006,27(5):366.
[10]	孙春华,黄建权,刘志鹏,等. HPLC-MS/MS快速同时测定全血中3种免疫抑制剂的浓度[J].中国药学杂志,2008,43(21):1643.

[1]	迟文雅, 袁艳, 李伟林, 吴茼妤, 俞媛. 负载骨髓间充质干细胞/白藜芦醇脂质体的水凝胶支架治疗创伤性脑损伤的研究 . 药学实践与服务, 2025, 43(2): 67-74. doi: 10.12206/j.issn.2097-2024.202406034
[2]	刘琳琳, 钟桂香, 严佳, 周欣. 不同使用条件下固相萃取柱对复方甘草口服溶液吗啡含量测定的影响 . 药学实践与服务, 2025, 43(12): 598-601. doi: 10.12206/j.issn.2097-2024.202311012
[3]	史生辉, 刘潇, 陈栋, 暨迪军, 马倩, 卢永昌. 二维液相色谱法分离藏药木藤蓼的化学成分 . 药学实践与服务, 2025, 43(9): 443-448. doi: 10.12206/j.issn.2097-2024.202412065
[4]	柯刚, 董清科, 肖世容, 龚茜, 李荣, 汪代杰. 基于网络药理学探讨参苓白术散治疗肿瘤恶病质的作用机制 . 药学实践与服务, 2025, 43(5): 242-250. doi: 10.12206/j.issn.2097-2024.202208115
[5]	曹奇, 张嘉宝, 王培. 基于无监督自动降维分析与手动圈门联用的骨骼肌髓系细胞多色流式分析方法 . 药学实践与服务, 2025, 43(7): 325-328, 366. doi: 10.12206/j.issn.2097-2024.202404077
[6]	黄欣, 杨茹洁, 秦峰, 张士莲, 吴莘, 尹小燕. 硫酸镁钠钾口服液在内镜肠道清洁准备中的效果 . 药学实践与服务, 2025, 43(): 1-4. doi: 10.12206/j.issn.2097-2024.202311049
[7]	俞千雪, 胡永胜, 黄艳秋, 丘炜桉, 陈啸飞, 李镐, 刘悦. 质谱成像技术在肝癌诊断与分子机制研究中的应用 . 药学实践与服务, 2025, 43(): 1-6. doi: 10.12206/j.issn.2097-2024.202411006
[8]	舒飞, 孙蕊, 宋凯, 张元林, 闫家铭, 舒丽芯. 粉-液双室袋产品的综合评价 . 药学实践与服务, 2025, 43(2): 92-96. doi: 10.12206/j.issn.2097-2024.202312009
[9]	彭莹, 刘欣, 聂依文, 王歆荷, 年华, 朱建勇. 三种狼毒乙醇提取物对咪喹莫特诱导的银屑病小鼠防治作用研究 . 药学实践与服务, 2025, 43(): 1-6. doi: 10.12206/j.issn.2097-2024.202406029
[10]	孟园园, 吴芸杨, 陈婷如, 顾秦五风, 杨延龙. 九味永安颗粒联合西替利嗪治疗湿疹湿热蕴肤证的临床疗效观察 . 药学实践与服务, 2025, 43(6): 298-302. doi: 10.12206/j.issn.2097-2024.202407045
[11]	吴海韵, 杨甜, 张弛, 梁文仪, 苏娟. 气相色谱-离子迁移谱技术在中药研究中的应用进展 . 药学实践与服务, 2025, 43(): 1-6. doi: 10.12206/j.issn.2097-2024.202409007
[12]	詹济华, 颜滢. 低蛋白血症对头孢哌酮舒巴坦血药浓度的影响 . 药学实践与服务, 2025, 43(7): 344-347. doi: 10.12206/j.issn.2097-2024.202309040
[13]	赵雪, 顾妍秋, 楚皓文, 吴彩胜, 李镐, 陈啸飞. 基于超高效液相色谱-四极杆飞行时间质谱的麻杏石甘汤化学成分分析 . 药学实践与服务, 2025, 43(11): 548-554, 571. doi: 10.12206/j.issn.2097-2024.202306028
[14]	黄雯婷, 刘志宏, 黄爱文, 张敏新, 宋洪涛. 西罗莫司自微乳-介孔硅缓释片的质量及体外释药行为考察 . 药学实践与服务, 2025, 43(11): 560-563. doi: 10.12206/j.issn.2097-2024.202402031
[15]	夏哲炜, 曾垣烨, 朱海菲, 李育, 陈啸飞. 核磁共振磷谱法测定磷酸氢钙咀嚼片中药物含量 . 药学实践与服务, 2024, 42(9): 399-401, 406. doi: 10.12206/j.issn.2097-2024.202404063
[16]	赖立勇, 夏天爽, 徐圣焱, 蒋益萍, 岳小强, 辛海量. 中药青蒿抗氧化活性的谱效关系研究 . 药学实践与服务, 2024, 42(5): 203-210, 216. doi: 10.12206/j.issn.2097-2024.202211012
[17]	陈春娟, 郑志新, 李骊. 平喘方联合孟鲁司特钠治疗儿童支气管哮喘的临床疗效观察 . 药学实践与服务, 2024, 42(12): 524-527, 532. doi: 10.12206/j.issn.2097-2024.202405035
[18]	丁千雪, 尚圣兰, 余梦辰, 余爱荣. 机器学习在肾病综合征患者他克莫司个体化用药中的应用 . 药学实践与服务, 2024, 42(6): 227-230, 243. doi: 10.12206/j.issn.2097-2024.202310007
[19]	桂明珠, 李静, 李志玲. 儿童伏立康唑的血药浓度与CYP2C19、CYP2C9和CYP3A5基因多态性的相关性研究 . 药学实践与服务, 2024, 42(): 1-5. doi: 10.12206/j.issn.2097-2024.202402020

点击查看大图

计量

文章访问数: 3537
HTML全文浏览量: 344
PDF下载量: 378
被引次数: 0

UPLC-MS/MS测定beagle犬内西罗莫司血药浓度

1. 福州大学化学化工学院 ,福建福州 350002;福建卫生职业技术学院,福建福州 350101

2. 福建省药品检验所,福建福州 350025

3. 南京军区福州总医院药学科,福建福州 350025

4. 福州大学化学化工学院 ,福建福州 350002

收稿日期: 2010-10-10
修回日期: 2011-03-31

关键词:

西罗莫司 /

超高效液相色谱-质谱联用 /

血药浓度

摘要: 目的建立测定beagle犬内西罗莫司(SRL)血药浓度的UPLC-MS/MS联用方法。方法色谱柱为Agilent C₁₈柱(50 mm × 2.1 mm,1.7 μm,);预柱为C₁₈柱(4.0 mm × 3.0 mm,5 μm);流动相为乙腈-水(90:10,v/v);流速为 0.30 ml/min;柱温为50℃;进样室温度为4 ℃。离子源为ESI源;正离子方式检测;扫描方式为多反应监测(MRM);用于定量分析的离子反应分别为m/z 936.6→m/z 409.7(西罗莫司)和m/z 826.6→m/z 415.4(内标他克莫司)。取全血样品经液-液萃取后进样20 μl。结果 SRL在0.50~12.00 ng/ml浓度范围内呈良好的线性(r=0.999 7),定量下限0.5 ng/ml,日内、日间精密度(RSD)均小于15%,方法回收率均大于90%,萃取回收率大于76%。结论本方法具有样品处理简单,方法灵敏、快速、选择性强,满足西罗莫司在beagle犬体内药物检测的要求。

English Abstract

Determination of sirolimus in whole blood of beagle dog by UPLC-MS/MS

1. Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China;Fujian Medical College, Fuzhou 350101, China

2. Fujian institute for Drug Control, Fuzhou 350025, China

3. Deptment of Pharmacy, Fuzhou General Hospital of Nanjing Military Command, Fuzhou 350025, China

4. Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China

Received Date: 2010-10-10
Rev Recd Date: 2011-03-31

Keywords:

sirolimus /
UPLC-MS/MS /
whole blood

Abstract: Objective To develop a UPLC-MS/MS method for the determination of sirolimus in whole blood of beagle dog. Methods Sirolimus and internal standard Tacrolimus were extracted from whole blood with liquid-liquid extraction,then separated on a Agilent C₁₈ column (50 mm ×2.1 mm,1.7 μm) at the flow-rate of 0.30 ml/min. The mobile phase was Acetonitrile-water (90∶10) and the column temperature was 50 ℃. Electrospray ionization ( ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 936.6→409.7 and m/z 826.6→415.4 were used to quantify sirolimus and the internal standard,respectively. Results The calibration linea range of blood-Sirolimu concentrations was 0.50~12.00 ng/ml(r=0.999 7).The low limit of quantification was 0.50 ng/ml . The intra-and inter-day precisions (RSDs) were less than 15%. The method recoveries were more than 90% . The extraction recoveries were more than 76%. Conclusions The method was specific,sensitive,rapid and suitable for the pharmacokinetic study of sirolimus in whole blood of beagle dog.

陈咏, 林晨, 张晶, 邱彬, 周欣, 宋洪涛. UPLC-MS/MS测定beagle犬内西罗莫司血药浓度[J]. 药学实践与服务, 2011, 29(5): 353-355,375.

引用本文:

陈咏, 林晨, 张晶, 邱彬, 周欣, 宋洪涛. UPLC-MS/MS测定beagle犬内西罗莫司血药浓度[J]. 药学实践与服务, 2011, 29(5): 353-355,375.

Citation: