GC-MS对多西他赛原料药中DMAP和DCC的残留检测

杜毅; 陈磊; 李玲; 周瑾; 吕磊

doi:10.3969/j.issn.1006-0111.2018.05.014

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GC-MS对多西他赛原料药中DMAP和DCC的残留检测

杜毅, 陈磊, 李玲, 周瑾, 吕磊

文章导航 > 药学实践与服务 > 2018 > 36(5): 446-449

杜毅, 陈磊, 李玲, 周瑾, 吕磊. GC-MS对多西他赛原料药中DMAP和DCC的残留检测[J]. 药学实践与服务, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

引用本文:

杜毅, 陈磊, 李玲, 周瑾, 吕磊. GC-MS对多西他赛原料药中DMAP和DCC的残留检测[J]. 药学实践与服务, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

DU Yi, CHEN Lei, LI Ling, Zhou Jin, LÜ Lei. Residue detection of DMAP and DCC in docetaxel by GC-MS[J]. Journal of Pharmaceutical Practice and Service, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

Citation:

DU Yi, CHEN Lei, LI Ling, Zhou Jin, LÜ Lei. Residue detection of DMAP and DCC in docetaxel by GC-MS[J]. Journal of Pharmaceutical Practice and Service, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

GC-MS对多西他赛原料药中DMAP和DCC的残留检测

doi: 10.3969/j.issn.1006-0111.2018.05.014

杜毅¹,
陈磊²,
李玲³,
周瑾⁴,
吕磊^4,

1.
上海交通大学医学院附属新华医院药学部, 上海 200092
2.
上海长海医院药材科, 上海 200433
3.
第二军医大学药学院分析测试中心, 上海 200433
4.
上海东方肝胆外科医院药材科, 上海 200438

Residue detection of DMAP and DCC in docetaxel by GC-MS

DU Yi¹,
CHEN Lei²,
LI Ling³,
Zhou Jin⁴,
LÜ Lei^4
,

1.
Department of Pharmacy, Xinhua Hospital Affiliated to School of Medicine, Shanghai Jiaotong University, Shanghai 200092, China
2.
Department of Pharmacy, Shanghai Changhai Hospital, Shanghai 200433, China
3.
Pharmaceutical Analysis Center, School of Pharmacy, Second Military Medical University, Shanghai 200433, China
4.
Department of Pharmacy, Shanghai Eastern Hepatobiliary Surgery Hospital, Shanghai 200438, China

摘要: 目的采用GC-MS技术对多西他赛原料药中催化剂4-二甲氨基吡啶（DMAP）和脱水剂二环己基碳二亚胺（DCC）进行残留检测。方法色谱柱为安捷伦的DB-5msUI（30 m×0.25 mm，0.25 μm）超高惰性毛细管气相色谱柱；采用程序升温方式，载气为高纯氦气，流速1.5 ml/min；进样量为1 μl。质谱采用EI源，选择离子监测模式：DMAP的定量离子为121，DCC的定量离子为163，内标龙脑的定量离子为95。多西他赛原料药采用甲醇超声提取。结果 DMAP和DCC的线性关系良好（r>0.999 2），其定量限分别为50.90和10.21 ng/ml，日内、日间精密度RSD均小于5.0%，回收率大于90%，符合方法学要求。3批样品中均未检测到DMAP和DCC的残留。结论该方法灵敏度高，专属性好，可用于多西他赛原料药中微量杂质的残留检测。
- 气相色谱-质谱联用 /
- 多西他赛 /
- 4-二甲氨基吡啶 /
- 二环己基碳二亚胺 /
- 残留检测
Abstract: Objective To establish a GC-MS method for residue detection of 4-Dimethylaminopyridine (DMAP) and Dicyclohexyl Carbodiimide (DCC) in docetaxel. Methods The separation was performed on an Agilent DB-5msUI capillary column (30 m×0.25 mm, 0.25 μm) with programmed temperature. The carrier gas was high purity helium, the flow rate was 1.5 ml/min and the injection volume was 1 μl. Electron impact ion source (EI) and selection monitoring mode (SIM) were applied for quantitative analysis. The quantitative ion of DMAP, DCC and internal standard (IS) was 121, 163 and 95 respectively. Docetaxel was ultrasonically extracted with methanol. Results The calibration of DMAP and DCC showed good linear relationship (r>0.999 2), the limits of quantification (LOQ) were 50.90 ng/ml and 10.21 ng/ml separately. Intra-day and inter-day precision were all less than 5% and recoveries were more than 90%, which conformed with the requirement of methodology validation. No residues of DMAP and DCC were detected in three batches of samples. Conclusion The method was sensitive and selective which can be used for the detection of trace impurities in docetaxel.
- GC-MS /
- docetaxel /
- DMAP /
- DCC /
- residue detection

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GC-MS对多西他赛原料药中DMAP和DCC的残留检测

doi: 10.3969/j.issn.1006-0111.2018.05.014

1. 上海交通大学医学院附属新华医院药学部, 上海 200092

2. 上海长海医院药材科, 上海 200433

3. 第二军医大学药学院分析测试中心, 上海 200433

4. 上海东方肝胆外科医院药材科, 上海 200438

收稿日期: 2018-03-07
修回日期: 2018-04-13

关键词:

摘要: 目的采用GC-MS技术对多西他赛原料药中催化剂4-二甲氨基吡啶（DMAP）和脱水剂二环己基碳二亚胺（DCC）进行残留检测。方法色谱柱为安捷伦的DB-5msUI（30 m×0.25 mm，0.25 μm）超高惰性毛细管气相色谱柱；采用程序升温方式，载气为高纯氦气，流速1.5 ml/min；进样量为1 μl。质谱采用EI源，选择离子监测模式：DMAP的定量离子为121，DCC的定量离子为163，内标龙脑的定量离子为95。多西他赛原料药采用甲醇超声提取。结果 DMAP和DCC的线性关系良好（r>0.999 2），其定量限分别为50.90和10.21 ng/ml，日内、日间精密度RSD均小于5.0%，回收率大于90%，符合方法学要求。3批样品中均未检测到DMAP和DCC的残留。结论该方法灵敏度高，专属性好，可用于多西他赛原料药中微量杂质的残留检测。

English Abstract

Residue detection of DMAP and DCC in docetaxel by GC-MS

1. Department of Pharmacy, Xinhua Hospital Affiliated to School of Medicine, Shanghai Jiaotong University, Shanghai 200092, China

2. Department of Pharmacy, Shanghai Changhai Hospital, Shanghai 200433, China

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

4. Department of Pharmacy, Shanghai Eastern Hepatobiliary Surgery Hospital, Shanghai 200438, China

Received Date: 2018-03-07
Rev Recd Date: 2018-04-13

Keywords:

GC-MS /
docetaxel /
DMAP /
DCC /
residue detection

Abstract: Objective To establish a GC-MS method for residue detection of 4-Dimethylaminopyridine (DMAP) and Dicyclohexyl Carbodiimide (DCC) in docetaxel. Methods The separation was performed on an Agilent DB-5msUI capillary column (30 m×0.25 mm, 0.25 μm) with programmed temperature. The carrier gas was high purity helium, the flow rate was 1.5 ml/min and the injection volume was 1 μl. Electron impact ion source (EI) and selection monitoring mode (SIM) were applied for quantitative analysis. The quantitative ion of DMAP, DCC and internal standard (IS) was 121, 163 and 95 respectively. Docetaxel was ultrasonically extracted with methanol. Results The calibration of DMAP and DCC showed good linear relationship (r>0.999 2), the limits of quantification (LOQ) were 50.90 ng/ml and 10.21 ng/ml separately. Intra-day and inter-day precision were all less than 5% and recoveries were more than 90%, which conformed with the requirement of methodology validation. No residues of DMAP and DCC were detected in three batches of samples. Conclusion The method was sensitive and selective which can be used for the detection of trace impurities in docetaxel.

杜毅, 陈磊, 李玲, 周瑾, 吕磊. GC-MS对多西他赛原料药中DMAP和DCC的残留检测[J]. 药学实践与服务, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

引用本文:

杜毅, 陈磊, 李玲, 周瑾, 吕磊. GC-MS对多西他赛原料药中DMAP和DCC的残留检测[J]. 药学实践与服务, 2018, 36(5): 446-449. doi: 10.3969/j.issn.1006-0111.2018.05.014

Citation: