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

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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

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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.

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UPLC-MS/MS测定beagle犬内西罗莫司血药浓度

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

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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

English Abstract

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

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目录

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