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

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

应中央军委要求，2022年9月起，《药学实践杂志》将更名为《药学实践与服务》，双月刊，正文96页；2023年1月起，拟出版月刊，正文64页，数据库收录情况与原《药学实践杂志》相同。欢迎作者踊跃投稿！

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

[1]	徐少杰,袁建勇,周辉,等. 多西他赛合成工艺[J]. 科技导报, 2010, 28(13):82-86.
[2]	孟秀敏. 多西他赛联合卡培他滨治疗紫杉醇耐药乳腺癌患者40例[J]. 中国药业, 2013, 22(17):64-65.
[3]	黄和,李丕宏,张毅,等. 多西他赛联合奥沙利铂及氟尿嘧啶治疗晚期胃癌临床观察[J]. 浙江医学, 2011, 33(2):183-185.
[4]	朱庆华,张国兵. 多西他赛与奈达铂联合治疗晚期非小细胞肺癌的临床疗效观察[J]. 中国现代医生, 2015, 53(20):89-92.
[5]	孙继国,周自成,夏玲远. 4-二甲氨基吡啶(DMAP)在医药合成中的应用[J]. 沧州师范学院学报, 2014, 30(1):49-53.
[6]	WIKIPEDIA. DMAP. Wikipedia website (2016). (2016-09-18).[2018-03-07]. https://en.wikipedia.org/wiki/4-Dimethylaminopyridine.
[7]	SAVJANI JK, MULAMKATTIL S, VARIYA B, et al. Molecular docking, synthesis and biological screening of mefenamic acid derivatives as anti-inflammatory agents[J]. Eur J Pharmacol, 2017, 801:28-34.
[8]	薄采颖,毕良武,王玉民,等. DCC及其在有机合成中的应用[J]. 化工时刊, 2007, 21(10):4-6.
[9]	范小振,张小杰,徐宝军. 高效液相色谱法测定烯草酮合成废液中4-二甲氨基吡啶含量[J]. 化学研究与应用, 2015, 27(2):237-239.
[10]	刘义国,郝文明. 气相色谱法分析N,N'-二环己基碳二亚胺的纯度[J]. 山东化工, 1998, 27(5):39-40.

[1]	万立志, 王境焓, 吴春蓉, 李玲. 基于代谢组学技术的烟酰胺协同两性霉素B抑制白念珠菌的作用机制研究 . 药学实践与服务, 2024, 42(): 1-6. doi: 10.12206/j.issn.2097-2024.202307034
[2]	周菊香, 王双英, 佘建涛, 曾贤良, 张继红. 肾衰竭对乳腺癌患者多西他赛暴露和不良反应的影响 . 药学实践与服务, 2022, 40(6): 571-575. doi: 10.12206/j.issn.2097-2024.202203068
[3]	杜毅, 丁德英, 吕磊, 李玲. 基于GC-MS技术的金钱草干预结晶肾损伤小鼠血清代谢组学研究 . 药学实践与服务, 2019, 37(4): 332-336. doi: 10.3969/j.issn.1006-0111.2019.04.009
[4]	林莉莉, 黄爱文, 林美钦, 方婕, 沈钦勇, 宋洪涛. 替吉奥单药或联合铂类治疗晚期非小细胞肺癌患者疗效与安全性的Meta评价 . 药学实践与服务, 2019, 37(6): 563-570. doi: 10.3969/j.issn.1006-0111.2019.06.018
[5]	张开霞, 王朝明, 金永生. 2-(3,4-二甲氧基苯基)-4-氧代-4H-色烯-3-基乙酸酯的晶体结构及旋光性 . 药学实践与服务, 2018, 36(2): 170-172,179. doi: 10.3969/j.issn.1006-0111.2018.02.015
[6]	梁睿姝, 熊礼燕, 李玲, 张川. 气相色谱-质谱联用法测定蓍草中的脂溶性成分 . 药学实践与服务, 2016, 34(6): 526-529. doi: 10.3969/j.issn.1006-0111.2016.06.011
[7]	张广军, 林玲, 陈丽娜, 高保安, 陈建明. 聚乙二醇400 介导的多西他赛脂肪乳剂与多西他赛注射液的稀释稳定性研究 . 药学实践与服务, 2015, 33(2): 119-121,175. doi: 10.3969/j.issn.1006-0111.2015.02.006
[8]	王彦, 俞仲望, 陈思, 李玲, 朱臻宇. 气相色谱-质谱联用结合代谢组学方法研究不同极化状态下小胶质细胞的代谢差异 . 药学实践与服务, 2015, 33(3): 226-230. doi: 10.3969/j.issn.1006-0111.2015.03.009
[9]	陈俊, 周瑾, 何赟鑫, 冯春华, 张国庆. 青风藤中挥发油成分的分析 . 药学实践与服务, 2012, 30(2): 115-117. doi: 10.3969/j.issn.1006-0111.2012.02.010
[10]	吕磊, 李玲, 田文君, 张海, 李悦悦, 张国庆, 赵亮. 中药复方扶正平消胶囊挥发油成分的GC-MS分析 . 药学实践与服务, 2012, 30(5): 353-356. doi: 10.3969/j.issn.1006-0111.2012.05.010
[11]	郭黎安, 王淑萍, 向丽, 姜鹏, 张卫东, 柳润辉. 气相色谱-质谱法定性分析麝香保心丸挥发性入血成分的研究 . 药学实践与服务, 2012, 30(3): 207-210. doi: 10.3969/j.issn.1006-0111.2012.03.013
[12]	温燕, 闻俊, 陶霞. 顶空气相色谱法测定奥利司他中残留溶剂 . 药学实践与服务, 2010, 28(3): 201-202.
[13]	刘职瑞, 刘文庸, 吴豪, 朱臻宇, 柴逸峰. 水蒸气蒸馏与乙醚超声萃取牡丹皮挥发油的比较研究 . 药学实践与服务, 2010, 28(4): 265-266,270.
[14]	吴玮峰, 杨志辉, 但志刚, 薛云云, 胡宏岗, 柴晓云, 俞世冲, 吴秋业. 1-(1H-1,2,4-三唑-1-基)-(2,4-二氟苯基)-3-(N-环己基-N-取代氨基)-2-丙醇的合成及抗真菌活性 . 药学实践与服务, 2009, 27(4): 266-269.
[15]	刘娜, 吕加国, 周有骏, 朱驹. L-2-(N-叔丁氧酰基)-3′,4′-二甲氧基苯丙氨酸乙酯的合成 . 药学实践与服务, 2009, 27(6): 445-447.
[16]	蔡林, 晏菊姣, 李恒. 顶空毛细管气相色谱法检测加替沙星中有机溶剂残留量 . 药学实践与服务, 2009, 27(5): 365-366,387.
[17]	李香, 林秀丽. 多西他赛与β-环糊精及羟丙基-β-环糊精包合作用的研究 . 药学实践与服务, 2008, (2): 129-133.
[18]	徐俊, 姜骏, 鲁莹. HPLC测定聚对二甲苯覆膜胶塞中二聚对二甲苯的残留量 . 药学实践与服务, 2007, (4): 235-237.
[19]	徐嵘. 多西他赛不同给药方案治疗非小细胞肺癌的效果 . 药学实践与服务, 2007, (4): 200-202,218.
[20]	张佳佳, 刘梅, 张文惠. 固相微萃取/气-质联用/选择离子检测法检测卷烟添加剂中的补骨脂 . 药学实践与服务, 2003, (6): 347-349.

点击查看大图

计量

文章访问数: 3701
HTML全文浏览量: 648
PDF下载量: 513
被引次数: 0

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:

全文HTML

参考文献 (10)

下载: 全尺寸图片幻灯片

返回文章

用微信扫码二维码

分享至好友和朋友圈

主管、主办: 中国人民解放军海军军医大学地址: 上海市杨浦区国和路325号邮政编码: 200433

电话: （021）81871324,81871397 E-mail: yxsjzzs@163.com

网站备案号沪ICP备05003363号-1

本系统由北京仁和汇智信息技术有限公司开发

留言板

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

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

计量

出版历程

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

English Abstract

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

全文HTML

目录

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