Establishment and performance evaluation of LC-MS/MS for the determination of plasma paclitaxel

doi:10.3969/j.issn.1673-8640.2016.05.012

Abstract

Abstract:

Objective To establish a liquid chromatography-tandem mass spectrometry（LC-MS/MS）for the quantitative determination of plasma paclitaxel,and to evaluate its performance. Methods Plasma paclitaxel was determined quantitatively by LC-MS/MS. High performance liquid chromatography was used. The flow speed was 0.3 mL/min. Multiple reaction monitoring （MRM） was used for quantitative determination. The ion pairs of paclitaxel and PTX-D5 were 876.4>308.2 and 881.5>313.2,respectively. According to U.S. Food and Drug Administration （FDA） guideline about bioanalytical method validation,the general analytical performance validation was performed for linearity,detection limit,precision and accuracy. Results The linearity was 10-1 000 ng/mL. The detection limit was 10 ng/mL. Within-run and between-run coefficients of variation （CV） were ≤4.2% and ≤8.9%,respectively. The accuracy was 88.7%-104.0%. Conclusions The performance of established LC-MS/MS meets evaluation standards,and the assay is accurate and precise for the determination of paclitaxel.

Key words: Paclitaxel, Liquid chromatography-tandem mass spectrometry, Analytical performance validation

CLC Number:

R446.1

WANG Kouqiong, SHAO Wenqi, PENG Yingfei, HUANG Fei, CHEN Fangjun, WU Jiong, WANG Beili, ZHANG Chunyan, GUO Wei, PAN Baishen. Establishment and performance evaluation of LC-MS/MS for the determination of plasma paclitaxel[J]. Laboratory Medicine, 2016, 31(5): 394-398.

Figures/Tables 6

References 7

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理论值（ng/mL）	测定值1（ng/mL）	测定值2（ng/mL）	均值（ng/mL）	DEV（%）
10	10.8	10.2	10.5	5.0
20	18.2	22.8	20.5	2.5
100	98.8	90.7	94.8	-5.2
250	265.7	215.6	240.7	-3.7
500	470.0	525.0	497.5	-0.5
1 000	1 016.5	1 015.7	1 016.1	1.6

理论值（ng/mL）	测定值1（ng/mL）	测定值2（ng/mL）	均值（ng/mL）	DEV（%）
10	10.8	10.2	10.5	5.0
20	18.2	22.8	20.5	2.5
100	98.8	90.7	94.8	-5.2
250	265.7	215.6	240.7	-3.7
500	470.0	525.0	497.5	-0.5
1 000	1 016.5	1 015.7	1 016.1	1.6

理论值（ng/mL）	实测值（ng/mL）					均值（ng/mL）	s （ng/mL）	CV （%）	S/N
理论值（ng/mL）	1	2	3	4	5	均值（ng/mL）	s （ng/mL）	CV （%）	S/N
10	11.9	10.4	11.1	11.6	11.9	11.4	0.64	5.6	774
20	19.7	18.2	22.8	19.2	21.8	20.3	1.9	9.4	1 501
100	92.5	98.8	90.7	113.6	110.7	101.3	10.4	10.3	5 006
250	233.9	265.7	215.6	240.4	232.7	237.7	18.2	7.6	7 490
500	482.7	470.0	525.0	514.3	527.4	503.9	26.0	5.2	8 929
1 000	1 039.7	1 016.5	1 015.7	983.2	979.1	1 006.8	25.4	2.5	9 102

理论值（ng/mL）	实测值（ng/mL）					均值（ng/mL）	s （ng/mL）	CV （%）	S/N
理论值（ng/mL）	1	2	3	4	5	均值（ng/mL）	s （ng/mL）	CV （%）	S/N
10	11.9	10.4	11.1	11.6	11.9	11.4	0.64	5.6	774
20	19.7	18.2	22.8	19.2	21.8	20.3	1.9	9.4	1 501
100	92.5	98.8	90.7	113.6	110.7	101.3	10.4	10.3	5 006
250	233.9	265.7	215.6	240.4	232.7	237.7	18.2	7.6	7 490
500	482.7	470.0	525.0	514.3	527.4	503.9	26.0	5.2	8 929
1 000	1 039.7	1 016.5	1 015.7	983.2	979.1	1 006.8	25.4	2.5	9 102

样本	批内		批间
样本	均值（ng/mL）	CV（%）	均值（ng/mL）	CV（%）
1	31.2	3.4	30.3	6.8
2	371.8	4.2	393.4	8.9
3	709.9	3.8	746.7	7.2