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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 Δ

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黄翠云 ，张 凤 ，柳 珂 ，陈万生 ，杨 军 （1.宜春学院化学与生物工程学院，江西 宜春 336000；2.解放军
第二军医大学长征医院药学部，上海 200003；3.解放军第二军医大学长征医院肿瘤科，上海 200003）
中图分类号 R969 文献标志码 A 文章编号 1001-0408（2020）01-0086-05
DOI 10.6039/j.issn.1001-0408.2020.01.15

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（r ＝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、
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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。
关键词 液相色谱-质谱联用；肿瘤患者；腹水；紫杉醇；含量测定

Determination of Paclitaxel in Malignant Ascites of Tumor Patients by LC-MS/MS
HUANG Cuiyun ，ZHANG Feng ，LIU Ke ，CHEN Wansheng ，YANG Jun （1.Chemistry and Biological
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Engineering College，Yichun University，Jiangxi Yichun 336000，China；2.Dept. of Pharmacy，Changzheng
Hospital， Second Military Medical University of PLA， Shanghai 200003， China；3.Dept. of Oncology，
Changzheng Hospital，Second Military Medical University of PLA，Shanghai 200003，China）
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
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range of paclitaxel were 25-2 500 ng/mL（r ＝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.
KEYWORDS LC-MS/MS；Tumor patient；Malignant ascites；Paclitaxel；Content determination

恶性肿瘤已经成为全球较大的公共卫生问题之
Δ 基金项目：国家自然科学基金资助项目（No.81573793）；上海市
[1]
科学技术委员会科研计划项目（No.18401931600）；上海市临床药学重 一 。恶性腹水是由于恶性肿瘤病变引起腹腔脏壁层腹
点专科建设项目（No.2016-40044-002） 膜发生弥漫性病变而导致腹腔内液体异常增多的现象，
＊药师，硕士。研究方向：临床药学。E-mail：44192977@qq.com 是恶性肿瘤晚期常见的并发症，在40％～60％的恶性腹
# 通信作者：教授，硕士。研究方向：临床药学。E-mail：yj1961@
[2]
126.com 水中能找到脱落的恶性肿瘤细胞 。紫杉醇是具有抗癌

·86 · China Pharmacy 2020 Vol. 31 No. 1 中国药房 2020年第31卷第1期