首页|LC-MS/MS法测定肿瘤患者血浆中帕米帕利浓度

LC-MS/MS法测定肿瘤患者血浆中帕米帕利浓度

扫码查看
目的 建立液相色谱-质谱联用(LC-MS/MS)法测定肿瘤患者血浆中帕米帕利浓度的方法。方法 使用乙腈沉淀血浆蛋白,以呋塞米为内标,采用LC-MS/MS测定帕米帕利的血药浓度。采用GL Sciences ODS-4 色谱柱,以含 0。1%甲酸水溶液为流动相A,甲醇为流动相B,进行梯度洗脱,流速为0。25 mL·min-1,柱温35℃,进样量为2 μL;采用电喷雾离子源,负离子扫描,多反应监测模式,用于定量分析的帕米帕利离子对为m/z 297。3→253。1。结果 帕米帕利检测质量浓度的线性范围为 100~10 000 ng·mL-1(r=0。995 4),定量下限为100 ng·mL-1;批内和批间准确度在 92。0%~106。5%之间,批内和批间精密度均小于 8。3%,基质效应、稳定性、选择性、残留均符合指导原则要求。临床患者帕米帕利体内随机血药浓度在 330~1 693 ng·mL-1之间。结论 所建方法操作简便、快速,可用于帕米帕利的血药浓度测定。
Determination of pamiparib in plasma of cancer patients by LC-MS/MS method
Objective To establish a liquid chromatography-mass spectrometry(LC-MS/MS)method for the determination of pamidronate concentration in plasma of cancer patients.Methods Acetonitrile was used to precipitate plasma protein,and furosemide was used as the internal standard.The plasma concentration of pamiparib was determined by LC-MS/MS.GL Sciences ODS-4 chromatographic column was used for gradient elution.The mobile phase A was 0.1%formic acid aqueous solution,and the mobile phase B was methanol.The flow rate was 0.25 mL·min-1,the column temperature was 35℃,and the injection volume was 2 μL.Negative ion scanning was performed using an electrospray ion source in a multi-reaction monitoring mode.The pamiparib ion pair used for quantitative analysis was m/z 297.3→253.1.Results The linear range of pamiparib was 100~10 000 ng·mL-1(r=0.995 4),and the lower limit of quantification was 100 ng·mL-1.The intra-batch and inter-batch accuracies were between 92.0%and 106.5%,and the intra-batch and inter-batch precisions were less than 8.3%.The matrix effect,stability,selectivity and residue all meet the requirements of the guiding principles.The random plasma concentration of pamiparib in clinical patients was between 330~1 693 ng·mL-1.Conclusion The established method was simple and rapid,and can be used for the determination of plasma concentration of pamiparib.

PamiparibLC-MS/MSDetermination of blood concentration

陈世贤、梁笑笑、时海燕、张霈、林晓晴、黄欣

展开 >

山东中医药大学药学院,山东 济南 250355

山东第一医科大学第一附属医院<山东省千佛山医院>药学部,山东 济南 250014

山东第一医科大学药学院,山东 济南 250117

帕米帕利 液相色谱-质谱联用 血药浓度测定

白求恩·求索-药学科研能力建设项目(2022)

2024

药学研究
山东省药品检验所 山东省药学会

药学研究

CSTPCD
影响因子:0.653
ISSN:2095-5375
年,卷(期):2024.43(5)
  • 12