Establishment of a liquid chromatography-tandem mass spectrometry for the determination of plasma 3-methoxytyramine

doi:10.3969/j.issn.1673-8640.2017.011.024

Abstract

Abstract:

Objective To establish a liquid chromatography-tandem mass spectrometry（LC-MS/MS） for plasma 3-methoxytyramine（3-MT） determination. Methods The separation condition of LC-MS/MS（chromatographic column,column temperature and pH value）was improved. The linear range,recovery rate,precision,lower limit of quantitation and stability of LC-MS/MS were evaluated. Results 3-MT was separated by BEH HILIC chromatographic column using 3-MT-d4 as internal standard. The mobile phase consisted of 100 mmol/L ammonium formate aqueous solution（pH value was 3）and acetonitrile. The column temperature was 35 ℃. The linear range of 3-MT determination were 5-1 000 pg/mL. The limit of quantitation was 5 pg/mL. The inter-day and between-run coefficients of variation（CV） were <6% and <7%. The recovery rate was 97.1%-109.3%. As 3-MT was unstable in room temperature,it should be transported under 4 ℃. Conclusions A reliable LC-MS/MS for the determination of 3-MT has been established,with sensitivity and accuracy.

Key words: 3-Methoxytyramine, Liquid chromotography-tandem mass spectrometry, Pheochromocytoma

CLC Number:

R446.1

QIN Jiaqian, PENG Yingfei, CHEN Fangjun, SHAO Wenqi, WU Jiong, ZHANG Chunyan, WANG Beili, GUO Wei, PAN Baishen. Establishment of a liquid chromatography-tandem mass spectrometry for the determination of plasma 3-methoxytyramine[J]. Laboratory Medicine, 2017, 32(11): 1046-1050.

Figures/Tables 8

References 9

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检测阶段	时间	流速（mL/min）	流动相A（%）	流动相B（%）
1		0.45	5.00	95.00
2	1.00	0.45	30.00	70.00
3	2.00	0.45	30.00	70.00
4	3.00	0.45	40.00	60.00
5	5.00	0.45	5.00	95.00

检测阶段	时间	流速（mL/min）	流动相A（%）	流动相B（%）
1		0.45	5.00	95.00
2	1.00	0.45	30.00	70.00
3	2.00	0.45	30.00	70.00
4	3.00	0.45	40.00	60.00
5	5.00	0.45	5.00	95.00

分析物	转换离子对（m/z）	锥孔电压（kV）	碰撞能量（eV）
3-MT定性	151→119	30	15
3-MT定量	151→91	30	15
3-MT-d4定量	155→95	30	15

分析物	转换离子对（m/z）	锥孔电压（kV）	碰撞能量（eV）
3-MT定性	151→119	30	15
3-MT定量	151→91	30	15
3-MT-d4定量	155→95	30	15

3-MT （ng/mL）	反复冻融（%）	室温放置24 h （%）	自动进样器放置36 h （%）
11.9	6.8	23.7	0.5
18.6	5.5	29.3	0.2