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

重要提示

《药学实践与服务》杂志不接收生物战剂、毒剂相关内容的稿件。对于涉军信息类论文如需投稿，请务必投稿前电话或邮箱咨询。联系电话：021-81871323，邮箱：yxsjzzs@163.com。敬请谅解，谢谢配合！

《药学实践与服务》编辑部

免责声明

《药学实践与服务》杂志目前不收取审稿费、版面费、加急费等费用，如收到邮件声称是编辑部X编辑，要求加作者微信的，请谨防财产损失！编辑部用于作者校稿时微信绑定的邮件是通过yxsjzzs@163.com发送的，标题是《药学实践与服务》XML数字出版服务微信绑定，请区分开！

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]	俞千雪, 胡永胜, 黄艳秋, 丘炜桉, 陈啸飞, 李镐, 刘悦. 质谱成像技术在肝癌诊断与分子机制研究中的应用 . 药学实践与服务, 2025, 43(): 1-6. doi: 10.12206/j.issn.2097-2024.202411006
[2]	黄雯婷, 刘志宏, 黄爱文, 张敏新, 宋洪涛. 西罗莫司自微乳-介孔硅缓释片的质量及体外释药行为考察 . 药学实践与服务, 2025, 43(11): 560-563. doi: 10.12206/j.issn.2097-2024.202402031
[3]	孟园园, 吴芸杨, 陈婷如, 顾秦五风, 杨延龙. 九味永安颗粒联合西替利嗪治疗湿疹湿热蕴肤证的临床疗效观察 . 药学实践与服务, 2025, 43(6): 298-302. doi: 10.12206/j.issn.2097-2024.202407045
[4]	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, 2025, 43(4): 185-189. doi: 10.12206/j.issn.2097-2024.202401072
[5]	关欣怡, 杨宇洁, 闻俊. 不同场景下芬太尼类新精神活性物质检测研究进展 . 药学实践与服务, 2025, 43(11): 533-539. doi: 10.12206/j.issn.2097-2024.202308033
[6]	段虎, 周艳卿, 钱瑜琳, 赵亮. 某二级医院稳定期慢性阻塞性肺疾病患者吸入治疗依从性及其影响因素 . 药学实践与服务, 2025, 43(7): 362-366. doi: 10.12206/j.issn.2097-2024.202204094
[7]	曹奇, 张嘉宝, 王培. 基于无监督自动降维分析与手动圈门联用的骨骼肌髓系细胞多色流式分析方法 . 药学实践与服务, 2025, 43(7): 325-328, 366. doi: 10.12206/j.issn.2097-2024.202404077
[8]	邱彦, 吴浩, 董雅芬, 陈业, 王建, 金辉. 新型二氢卟吩化合物的光动力性能及其抗肺癌作用研究 . 药学实践与服务, 2025, 43(): 1-7. doi: 10.12206/j.issn.2097-2024.202304011
[9]	赵雪, 顾妍秋, 楚皓文, 吴彩胜, 李镐, 陈啸飞. 基于超高效液相色谱-四极杆飞行时间质谱的麻杏石甘汤化学成分分析 . 药学实践与服务, 2025, 43(11): 548-554, 571. doi: 10.12206/j.issn.2097-2024.202306028
[10]	史生辉, 刘潇, 陈栋, 暨迪军, 马倩, 卢永昌. 二维液相色谱法分离藏药木藤蓼的化学成分 . 药学实践与服务, 2025, 43(9): 443-448. doi: 10.12206/j.issn.2097-2024.202412065
[11]	吴海韵, 杨甜, 张弛, 梁文仪, 苏娟. 气相色谱-离子迁移谱技术在中药研究中的应用进展 . 药学实践与服务, 2025, 43(): 1-6. doi: 10.12206/j.issn.2097-2024.202409007
[12]	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
[13]	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
[14]	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
[15]	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
[16]	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
[17]	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
[18]	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(12): 528-532. doi: 10.12206/j.issn.2097-2024.202305005
[19]	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
[20]	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: 6352
HTML全文浏览量: 1009
PDF下载量: 609
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: