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Article Navigation >  Journal of Pharmaceutical Practice and Service  > 2018  >  36(5): 446-449

QIAO Liye, FANG Li, CAO Yanli, LU Yin, SU Hua, WANG Shudong. Determination of aloe-emodin,rhein,emodin,chrysophanol and physcion in Xinbaoshen tablets by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(5): 438-440. doi: 10.3969/j.issn.1006-0111.2015.05.015
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
shu

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

doi: 10.3969/j.issn.1006-0111.2018.05.014
  • 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
  • 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.
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    [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.
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Residue detection of DMAP and DCC in docetaxel by GC-MS

doi: 10.3969/j.issn.1006-0111.2018.05.014
  • 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

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.

QIAO Liye, FANG Li, CAO Yanli, LU Yin, SU Hua, WANG Shudong. Determination of aloe-emodin,rhein,emodin,chrysophanol and physcion in Xinbaoshen tablets by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2015, 33(5): 438-440. doi: 10.3969/j.issn.1006-0111.2015.05.015
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
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