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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（含0.1％甲酸和10 mmol/L 醋酸铵）-乙腈溶液（40 ∶ 60，V/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876.5→308.0、457.3→188.1，碎片电压分别为250、150 V，碰撞电压分别为30、20 eV。结果：紫杉醇检测质量浓度的 线性范围为25～2 500 ng/mL（r2＝0.996 5，n＝7）；定量下限为25 ng/mL；日内、日间精密度试验的RSD为0.61％～3.62％（n＝5、 3）；准确度为95.34％～98.76％（n＝5、3）；提取回收率的RSD为3.19％～3.72％（n＝3）；基质效应的CV为1.52％～2.93％（n＝3）； 稳定性试验的RE均小于3％（n＝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。
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| ABSTRACT： |
ABSTRACT OBJECTIVE：To establish a method for content determination of paclitaxel in malignant ascites of tumor patients.
METHODS：LC-MS/MS method was adopted. Using vindoline as internal standard，the 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 0.1％ formic acid and 10 mmol/L ammonium acetate）-acetonitrile（40 ∶ 60，V/V）at 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 source，and 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/min，capillary voltage 4 000 V. Quantitative determination was operated in the multiple reaction monitoring（MRM）mode， with the ion transitions m/z 876.5→308.0 for paclitaxel and m/z 457.3→188.1 for the internal standard. The fragment voltage/ collision energy for paclitaxel and the internal standard were 250 V/30 eV，and 150 V/20 eV，respectively. RESULTS：The linear range of paclitaxel were 25-2 500 ng/mL（r2＝0.996 5，n＝7）. The lowest limit of quantitation was 25 ng/mL. RSDs of inter-day and intra-day precision tests were 0.61％ -3.62％（n＝5，3）. Accuracies were 95.34％ -98.76％（n＝5，3）. RSDs of extraction recovery were 3.19％-3.72％（n＝3）. CV of matrix effect were 1.52％-2.93％（n＝3）. RE of stability tests were lower than 3％（n＝ 3）. CONCLUSIONS：The method is simple，accurate and suitable for the content determination of paclitaxel in malignant ascites of tumor patients.
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| 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 |
| 阅读数： | 435 次 |
| 本月下载数： | 15 次 |
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