HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

王晶; 董昕; 邹豪; 金磊; 张川

doi:10.3969/j.issn.1006-0111.2012.01.014

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HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

王晶, 董昕, 邹豪, 金磊, 张川

文章导航 > 药学实践与服务 > 2012 > 30(1): 52-54

王晶, 董昕, 邹豪, 金磊, 张川. HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度[J]. 药学实践与服务, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

引用本文:

王晶, 董昕, 邹豪, 金磊, 张川. HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度[J]. 药学实践与服务, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

WANG Jing, DONG Xin, ZOU Hao, JIN Lei, ZHANG Chuan. Determination of sodium Danshensu in rat liver by HPLC-MS/MS[J]. Journal of Pharmaceutical Practice and Service, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

Citation:

WANG Jing, DONG Xin, ZOU Hao, JIN Lei, ZHANG Chuan. Determination of sodium Danshensu in rat liver by HPLC-MS/MS[J]. Journal of Pharmaceutical Practice and Service, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

doi: 10.3969/j.issn.1006-0111.2012.01.014

王晶¹,
董昕²,
邹豪³,
金磊³,
张川^3,

1.
第二军医大学药学院新药研究中心,上海 200433;上海市中山医院青浦分院药剂科,上海 201700
2.
第二军医大学药学院分析测试中心,上海 200433
3.
第二军医大学药学院新药研究中心,上海 200433

基金项目: 上海市中药现代化专项基金(08DZ1970802).

Determination of sodium Danshensu in rat liver by HPLC-MS/MS

1.
New drug research center, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Deportment of pharmacy,Qingpu Distric Central Hosptal,Shanghai 201700, China
2.
Center of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China
3.
New drug research center, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

摘要: 目的建立液质联用色谱法(HPLC-MS/MS)测定SD大鼠肝脏组织中丹参素钠的浓度。方法肝脏组织样品制成匀浆后,加入内标酮洛芬,采用液液萃取方法进行预处理。色谱柱:Diamonsil C₁₈柱(200 mm×4.6 mm ,5 μm);流动相:甲醇-水(含0.01‰甲酸)(80:20);流速:1.0 ml/min;质谱条件:采用ESI离子源,负离子检测,选择MRM 测定丹参素钠和酮洛芬197→135 m/z 和 253→209 m/z。结果丹参素钠在20.2~1 010 n
- 液质联用色谱法 /
- 丹参素钠 /
- 组织浓度
Abstract: Objective To establish a HPLC-MS/MS method for determination of sodium Danshensu in SD rat liver. Methods Tissue samples were pretreated by liquid-liquid extraction method after homogenate, and ketoprofen was used as the internal standard. Analytical column was Diamonsil C₁₈ (200 mm×4.6 mm, 5 μm). The mobile phase was methanol: water(0.01‰ formic acid)=80:20 with flow rate as 1.0 ml/min. Mass spectrum determination was performed in the MRM mode with target ions m/z 197→135 (Sodium Danshensu), m/z 253→209 (ketoprofen), using ESI ion resource and negative ion detection. Results The calibration curve was linear over the range of 20.2~1 010 ng/ml. The LLOQ of sodium Danshensu in liver was 20.2 ng/ml. The intra-and inter-day RSD were both less than 10%. The extracted recovery rate ranged from 92% to 107%. Conclusion The method was sensitive, rapid, simple and accurate to determine sodium Danshensu distribution in rat liver and was suitable for preclinical test of Sodium Danshensu.
- HPLC-MS/MS /
- sodium Danshensu /
- drug concentration in tissue

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HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度

doi: 10.3969/j.issn.1006-0111.2012.01.014

1. 第二军医大学药学院新药研究中心,上海 200433;上海市中山医院青浦分院药剂科,上海 201700

2. 第二军医大学药学院分析测试中心,上海 200433

3. 第二军医大学药学院新药研究中心,上海 200433

基金项目: 上海市中药现代化专项基金(08DZ1970802).

收稿日期: 2011-04-21
修回日期: 2011-06-14

关键词:

液质联用色谱法 /

丹参素钠 /

组织浓度

摘要: 目的建立液质联用色谱法(HPLC-MS/MS)测定SD大鼠肝脏组织中丹参素钠的浓度。方法肝脏组织样品制成匀浆后,加入内标酮洛芬,采用液液萃取方法进行预处理。色谱柱:Diamonsil C₁₈柱(200 mm×4.6 mm ,5 μm);流动相:甲醇-水(含0.01‰甲酸)(80:20);流速:1.0 ml/min;质谱条件:采用ESI离子源,负离子检测,选择MRM 测定丹参素钠和酮洛芬197→135 m/z 和 253→209 m/z。结果丹参素钠在20.2~1 010 n

English Abstract

Determination of sodium Danshensu in rat liver by HPLC-MS/MS

1. New drug research center, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Deportment of pharmacy,Qingpu Distric Central Hosptal,Shanghai 201700, China

2. Center of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

3. New drug research center, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

Received Date: 2011-04-21
Rev Recd Date: 2011-06-14

Keywords:

Abstract: Objective To establish a HPLC-MS/MS method for determination of sodium Danshensu in SD rat liver. Methods Tissue samples were pretreated by liquid-liquid extraction method after homogenate, and ketoprofen was used as the internal standard. Analytical column was Diamonsil C₁₈ (200 mm×4.6 mm, 5 μm). The mobile phase was methanol: water(0.01‰ formic acid)=80:20 with flow rate as 1.0 ml/min. Mass spectrum determination was performed in the MRM mode with target ions m/z 197→135 (Sodium Danshensu), m/z 253→209 (ketoprofen), using ESI ion resource and negative ion detection. Results The calibration curve was linear over the range of 20.2~1 010 ng/ml. The LLOQ of sodium Danshensu in liver was 20.2 ng/ml. The intra-and inter-day RSD were both less than 10%. The extracted recovery rate ranged from 92% to 107%. Conclusion The method was sensitive, rapid, simple and accurate to determine sodium Danshensu distribution in rat liver and was suitable for preclinical test of Sodium Danshensu.

王晶, 董昕, 邹豪, 金磊, 张川. HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度[J]. 药学实践与服务, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

引用本文:

王晶, 董昕, 邹豪, 金磊, 张川. HPLC-MS/MS 测定大鼠肝脏组织中丹参素钠的浓度[J]. 药学实践与服务, 2012, 30(1): 52-54. doi: 10.3969/j.issn.1006-0111.2012.01.014

Citation: