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]	黄韵, 张正银, 金英, 郑怡菁, 李铁军, 孙莉莉. 耐碳青霉烯类肺炎克雷伯菌及大肠埃希菌临床分离株耐药性及耐药基因分析 . 药学实践与服务, 2024, 42(10): 439-444. doi: 10.12206/j.issn.2097-2024.202309059
[2]	钱淑雨, 李铁军. 耐碳青霉烯类肠杆菌耐药机制的研究进展 . 药学实践与服务, 2024, 42(10): 419-425. doi: 10.12206/j.issn.2097-2024.202405005
[3]	景凯, 杨慈荣, 张圳, 臧艺蓓, 刘霞. 黄芪甲苷衍生物治疗慢性心力衰竭小鼠的药效评价及作用机制研究 . 药学实践与服务, 2024, 42(5): 190-197. doi: 10.12206/j.issn.2097-2024.202310004
[4]	刘汝雄, 杨万镇, 涂杰, 盛春泉. 铁死亡调控蛋白GPX4的小分子抑制剂研究进展 . 药学实践与服务, 2024, 42(9): 375-378. doi: 10.12206/j.issn.2097-2024.202312075
[5]	李丹, 戴贤春, 王芳珍, 陈奕含, 杨萍, 刘继勇. HPLC-MS/MS测定当归六黄汤中4种不同成分的含量 . 药学实践与服务, 2024, 42(6): 248-252, 266. doi: 10.12206/j.issn.2097-2024.202305007
[6]	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
[7]	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用于创伤性脑损伤治疗 . 药学实践与服务, 2024, 42(): 1-8. doi: 10.12206/j.issn.2097-2024.202406034
[8]	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
[9]	王鹏, 陈顺, 赵逸, 高守红, 王志鹏. 卡培他滨致小鼠手足综合征模型的建立及评价 . 药学实践与服务, 2024, 42(9): 385-388, 398. doi: 10.12206/j.issn.2097-2024.202308045
[10]	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
[11]	瞿文君, 白若楠, 崔力, 周琰. 基于联合库存的公立医院多院区药品采购模式分析 . 药学实践与服务, 2024, 42(7): 315-318. doi: 10.12206/j.issn.2097-2024.202401002
[12]	姚小静, 计佩影, 陆峰, 施国荣, 傅翔. 表面增强拉曼光谱法快速测定尿液中曲马多的研究 . 药学实践与服务, 2024, 42(): 1-5. doi: 10.12206/j.issn.2097-2024.202401072
[13]	顾佳钰, 胡馨儿, 王晓飞, 张颖, 张海, 曹岩. 侧流免疫层析定量检测方法的研究进展 . 药学实践与服务, 2024, 42(7): 273-277, 284. doi: 10.12206/j.issn.2097-2024.202307037
[14]	毛泽玲, 文波. 大黄的HPLC指纹图谱及禁用农药的残留研究 . 药学实践与服务, 2024, 42(7): 297-304, 314. doi: 10.12206/j.issn.2097-2024.202310057
[15]	戴菲菲, 傅翔, 陈琼年, 俞苏纯. 上海某二级医院革兰阴性菌流行特征的回顾性分析 . 药学实践与服务, 2024, 42(): 1-5. doi: 10.12206/j.issn.2097-2024.202305005
[16]	张艺昕, 关欣怡, 王博宁, 闻俊, 洪战英. 二氢吡啶类钙离子拮抗药物手性分析及其立体选择性药动学研究进展 . 药学实践与服务, 2024, 42(8): 319-324. doi: 10.12206/j.issn.2097-2024.202308062
[17]	毛智毅, 王筱燕, 陈晓颖, 汤逸斐. 度拉糖肽联合二甲双胍对肥胖型2型糖尿病患者机体代谢、体脂成分及血清脂肪因子的影响 . 药学实践与服务, 2024, 42(7): 305-309. doi: 10.12206/j.issn.2097-2024.202305032

点击查看大图

计量

文章访问数: 4702
HTML全文浏览量: 805
PDF下载量: 525
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: [email protected]

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