HPLC-ICP-MS Determination of Carboplatin and Chloroplatinic Acid
摘 要
称取样品0.100 0 g,用水溶解后,根据被测物浓度不同加水定量稀释至合适浓度。在高效液相色谱分离中,选择PRP-X100为分离柱,由于固定相上键合有二乙烯基苯/三乙胺聚合物,对氯铂酸和卡铂的分离效果较好。用60 mmol·L-1硝酸铵溶液(预先用稀氨水或稀硝酸调节其酸度至pH 5.5)为流动相,按等梯度程序进行洗脱。分离后的洗脱液按质谱仪器的工作条件进行测定。结果表明:氯铂酸和卡铂的线性范围依次为1.00~100 μg·L-1和500.0~1 000 μg·L-1;检出限(3S/N)依次为0.1,0.01 μg·L-1。按标准加入法在实际样品基础上进行回收试验,测得氯铂酸的回收率为90.0%~98.8%,卡铂的回收率为98.5%~99.2%,两者测定值的相对标准偏差(n=6)依次为2.7%~3.4%和2.1%~2.8%。应用上述方法进行实际样品分析时还发现,当卡铂的检测量为1 mg·L-1时,未检测到氯铂酸,故该方法无需富集就能达到痕量铂的测定。
Abstract
A portion of the sample (0.100 0 g) was dissolved in water and diluted to an appropriate volume according to the concentration of the analyte in sample. The ion-exchange column PRP-X100 was chosen as separation column, which was proved to have high efficiency in separation of chloroplatinic acid and carboplatin, due to bonding of polymer of divinylbenzene/triethylamine on the stationary phase. 60 mmol·L-1 NH4NO3 solution (pre-adjusted its acidity to pH 5.5 with dil. NH3·H2O or dil. HNO3) was used as mobile phase in the gradient elution program. Analyte in respective eluate was then determined by ICP-MS according to the prescribed procedure. As shown by the results, linearity ranges for chloroplatinic acid and carboplatin were found between 1.00 and 100 μg·L-1 and between 500.0 and 1 000 μg·L-1 with detection limits (3S/N) of 0.1 μg·L-1 and 0.01 μg·L-1respectively. Testes for recovery were performed by standard addition method using a substantial sample as matrix, giving values of recovery of 90.0%-98.8% for chloroplatinic acid and of 98.5%-99.2% for carboplatin. Values of RSDs (n=6) found was 2.7%-3.4% for chloroplatinic acid and 2.1%-2.8% for carbonplatin. It was found that in the analysis of a substantial sample by the proposed method, as the concentration of carboplatin found was 1 mg·L-1, H2[PtCl6] was not inspected in the same sample. Hence, inspection of traces of platinum(Ⅳ) was attained directly in the sample solution without any enrichment manipulation.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201907022
所属栏目 专题报道(电感耦合等离子体质谱法)
基金项目 北京市农林科学院创新建设项目(KJCX20170419)
收稿日期 2018/9/28
修改稿日期
网络出版日期
作者单位点击查看
备注李冰茹,工程师,硕士,研究方向为农产品质量检测及污染评价
引用该论文: LI Bingru,LIU Jing,YAO Zhenzhen,WANG Beihong,LI Qiang,FU Weili,MA Zhihong. HPLC-ICP-MS Determination of Carboplatin and Chloroplatinic Acid[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(7): 865~868
李冰茹,刘静,姚真真,王北洪,李强,付伟丽,马智宏. 高效液相色谱-电感耦合等离子体质谱法测定卡铂和氯铂酸的含量[J]. 理化检验-化学分册, 2019, 55(7): 865~868
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】还传静,李悦,陆静.铂类药物杂质及其检测方法的研究进展[J].中国药房, 2017,28(30):4315-4320.
【2】陈嘉彬,何蔓,陈贝贝,等.磁固相萃取与高效液相色谱-等离子体质谱联用检测癌症病人尿样中的卡铂药物[J].分析科学学报, 2014(5):607-612.
【3】黄品芳,刘亦伟,王长连.高效液相色谱法测定人血清卡铂浓度[J].福建医科大学学报, 2007,41(4):363-364.
【4】谢志红,叶丽卡,周龙书,等.高效液相色谱法测定人血浆中卡铂浓度[J].中国医院药学杂志, 2009,29(6):457-459.
【5】刘德晔,朱醇,马永建,等.高效液相色谱-电感耦合等离子体质谱测定血浆中铂类抗癌药物[J].分析试验室, 2012,31(7):75-79.
【6】谌喜珠,杨一昆,熊惠周,等.抗癌药物卡铂薄层色谱分析方法研究[J].贵金属, 1999,20(2):40-42.
【7】VIVEKANANDAN K, SWAMY M, PRASAD S, et al. Identification of degradation products from aqueous carboplatin injection samples by electrospray mass spectrometry[J]. International Journal of Pharmaceutics, 2006,313(1/2):214-221.
【8】杨叶梅,贺与平,陈金素,等.ICP-AES法测定顺铂、卡铂血药浓度[J].中国卫生检验杂志, 2000,10(3):259-261.
【9】张萍,杨慧,宋梅,等.RP-HPLC法测定卡铂制剂中卡铂的含量[J].中国药房, 2012,23(4):367-369.
【10】马张英,李文钧,裘飞君,等.高效液相色谱法测定卡铂粉针和水针剂的含量[J].中国医院药学杂志, 2004,24(4):247-248.
【11】FERNÁNDEZ-PERALBO M A, PRIEGO-CAPOTE F, LUQUE D C D, et al. LC-MS/MS quantitative analysis of paclitaxel and its major metabolites in serum, plasma and tissue from women with ovarian cancer after intraperitoneal chemotherapy[J]. Journal of Pharmaceutical and Biomedical Analysis, 2014,91:131-137.
【12】杜春双,陈琛,宋晓坤,等.卡铂注射液的含量测定及其临床使用稳定性研究[J].中国药房, 2011,22(5):442-444.
【13】SHU C, ZENG T M, GAO S H, et al. LC-MS/MS method for simultaneous determination of thalidomide, lenalidomide, cyclophosphamide, bortezomib, dexamethasone and adriamycin in serum of multiple myeloma patients[J]. Journal of Chromatography B, 2016,1028:111-119.
【14】GAO S H, TAO Z B, ZHOU J Y, et al. One-step solid extraction for simultaneous determination of eleven commonly used anticancer drugs and one active metabolite in human plasma by HPLC-MS/MS[J]. Journal of Analytical Methods in Chemistry, 2018,2018:1-12.
【15】VALE G, RODRIGUES A, ROCHA A, et al. Ultrasonic assisted enzymatic digestion (USAED) coupled with high performance liquid chromatography and electrothermal atomic absorption spectrometry as a powerful tool for total selenium and selenium species control in Se-enriched food supplements[J]. Food Chemistry, 2010,121(1):268-274.
【2】陈嘉彬,何蔓,陈贝贝,等.磁固相萃取与高效液相色谱-等离子体质谱联用检测癌症病人尿样中的卡铂药物[J].分析科学学报, 2014(5):607-612.
【3】黄品芳,刘亦伟,王长连.高效液相色谱法测定人血清卡铂浓度[J].福建医科大学学报, 2007,41(4):363-364.
【4】谢志红,叶丽卡,周龙书,等.高效液相色谱法测定人血浆中卡铂浓度[J].中国医院药学杂志, 2009,29(6):457-459.
【5】刘德晔,朱醇,马永建,等.高效液相色谱-电感耦合等离子体质谱测定血浆中铂类抗癌药物[J].分析试验室, 2012,31(7):75-79.
【6】谌喜珠,杨一昆,熊惠周,等.抗癌药物卡铂薄层色谱分析方法研究[J].贵金属, 1999,20(2):40-42.
【7】VIVEKANANDAN K, SWAMY M, PRASAD S, et al. Identification of degradation products from aqueous carboplatin injection samples by electrospray mass spectrometry[J]. International Journal of Pharmaceutics, 2006,313(1/2):214-221.
【8】杨叶梅,贺与平,陈金素,等.ICP-AES法测定顺铂、卡铂血药浓度[J].中国卫生检验杂志, 2000,10(3):259-261.
【9】张萍,杨慧,宋梅,等.RP-HPLC法测定卡铂制剂中卡铂的含量[J].中国药房, 2012,23(4):367-369.
【10】马张英,李文钧,裘飞君,等.高效液相色谱法测定卡铂粉针和水针剂的含量[J].中国医院药学杂志, 2004,24(4):247-248.
【11】FERNÁNDEZ-PERALBO M A, PRIEGO-CAPOTE F, LUQUE D C D, et al. LC-MS/MS quantitative analysis of paclitaxel and its major metabolites in serum, plasma and tissue from women with ovarian cancer after intraperitoneal chemotherapy[J]. Journal of Pharmaceutical and Biomedical Analysis, 2014,91:131-137.
【12】杜春双,陈琛,宋晓坤,等.卡铂注射液的含量测定及其临床使用稳定性研究[J].中国药房, 2011,22(5):442-444.
【13】SHU C, ZENG T M, GAO S H, et al. LC-MS/MS method for simultaneous determination of thalidomide, lenalidomide, cyclophosphamide, bortezomib, dexamethasone and adriamycin in serum of multiple myeloma patients[J]. Journal of Chromatography B, 2016,1028:111-119.
【14】GAO S H, TAO Z B, ZHOU J Y, et al. One-step solid extraction for simultaneous determination of eleven commonly used anticancer drugs and one active metabolite in human plasma by HPLC-MS/MS[J]. Journal of Analytical Methods in Chemistry, 2018,2018:1-12.
【15】VALE G, RODRIGUES A, ROCHA A, et al. Ultrasonic assisted enzymatic digestion (USAED) coupled with high performance liquid chromatography and electrothermal atomic absorption spectrometry as a powerful tool for total selenium and selenium species control in Se-enriched food supplements[J]. Food Chemistry, 2010,121(1):268-274.
相关信息