LC-MS/MS法测定肿瘤患者恶性腹水中紫杉醇的含量
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篇名: LC-MS/MS法测定肿瘤患者恶性腹水中紫杉醇的含量
TITLE:
摘要:
摘 要 目的建立测定肿瘤患者恶性腹水中紫杉醇含量的方法方法采用液相色谱-质谱联用LC-MS/MS技术以文多灵为 内标测定肿瘤患者给予紫杉醇后恶性腹水中紫杉醇的含量色谱柱为Zorbax SB-C18流动相为水溶液0.1甲酸和10 mmol/L 醋酸铵-乙腈溶液40 60V/V),流速为0.25 mL/min柱温为30 进样量为5 μL离子源为电喷雾离子源检测模式为多重反应 离子监测正离子模式干燥气温度为350 干燥气流速为10 L/min毛细管电压为4 000 V紫杉醇和内标在正离子模式下质荷比 m/z分别为876.5308.0457.3188.1碎片电压分别为250150 V碰撞电压分别为3020 eV结果紫杉醇检测质量浓度的 线性范围为25~2 500 ng/mLr2=0.996 5n=7);定量下限为25 ng/mL日内日间精密度试验的RSD0.61~3.62n=53);准确度为95.34~98.76n=53);提取回收率的RSD3.19~3.72n=3);基质效应的CV1.52~2.93n=3); 稳定性试验的RE均小于3n=3)。结论该方法简便准确可用于测定肿瘤患者恶性腹水中紫杉醇的含量
ABSTRACT:
ABSTRACT OBJECTIVETo establish a method for content determination of paclitaxel in malignant ascites of tumor patients.
METHODSLC-MS/MS method was adopted. Using vindoline as internal standardthe content of paclitaxel in ascites of tumor
patients was determined. The separation was performed on Zorbax SB-C18 column with mobile phase consisted of aqueous solution
containing 0.1formic acid and 10 mmol/L ammonium acetate-acetonitrile40 60V/Vat the flow rate of 0.25 mL/min. the column temperature was 30 and sample size was 5 μL. The ion source was electrospray ion sourceand the detection mode was multiple ion monitoring positive ion mode. MS parameters were set as following as dry gas temperature 350 dry gas flow rate 10 L/mincapillary voltage 4 000 V. Quantitative determination was operated in the multiple reaction monitoringMRMmodewith the ion transitions m/z 876.5308.0 for paclitaxel and m/z 457.3188.1 for the internal standard. The fragment voltage/ collision energy for paclitaxel and the internal standard were 250 V/30 eVand 150 V/20 eVrespectively. RESULTSThe linear range of paclitaxel were 25-2 500 ng/mLr2=0.996 5n=7. The lowest limit of quantitation was 25 ng/mL. RSDs of inter-day and intra-day precision tests were 0.61-3.62n=53. Accuracies were 95.34-98.76n=53. RSDs of extraction recovery were 3.19-3.72n=3. CV of matrix effect were 1.52-2.93n=3. RE of stability tests were lower than 3n3. CONCLUSIONSThe method is simpleaccurate and suitable for the content determination of paclitaxel in malignant ascites of tumor patients.
期刊: 2020年第31卷第1期
作者: 黄翠云,张 凤,柳 珂,陈万生,杨 军
AUTHORS: HUANG Cuiyun,ZHANG Feng,LIU Ke,CHEN Wansheng,YANG Jun
关键字: 液相色谱-质谱联用;肿瘤患者;腹水;紫杉醇;含量测定
KEYWORDS: LC-MS/MS;Tumor patient;Malignant ascites;Paclitaxel;Content determination
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