. Author manuscript; available in PMC: 2018 Aug 15.

Published in final edited form as: J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Jun 19;1060:316–324. doi: 10.1016/j.jchromb.2017.06.028

Table 1.

LC/MS determination of nitrogen mustard antineoplastic drugs in urine

Parent drug	Sample preparation	Chromatography	Interface/Detection	Target analyte	m/z of mass transition	Limit of Detection	Reference
cyclophosphamide (CP)	LLE ethylacetate	RP C8/isocratic CH₃CO₂NH₄/MeOH 4.6 × 150 mm, 5μm	ESI/QQQ/MRM⁺	CP IF	261.2/140.2 261.2/92.0	0.05 μg/L	[21]
cyclophosphamide	LLE ethylacetate	RP C18/gradient CH₃COOH/MeOH 2.1 × 50 mm, 4μm	ESI/QQQ/MRM⁺	CP d₆-CP	263.1/142.1 267.1/140.3	0.01 μg/L	[22]
cyclophosphamide	SPE C18 ethylacetate	RP C18/gradient HCO₂NH₄/ACN 3.0 × 150 mm, 3μm	ESI⁺/QTrap	CP d₄-CP	261/140 265/140	0.05 μg/L	[23]
cyclophosphamide	SPE C18 ethylacetate/dichloromethane	RP C18/isocratic CH₃COOH/ACN 3.0 × 100 mm, 2.7μm	ESI/QQQ/MRM⁺	CP IF	261/140 261/54	0.07 μg/L	[24]
cyclophosphamide ifosphamide (IF)	salt-assisted LLE ethylacetate sodium borate	RP C8/isocratic HCOOH/ACN 2.0 × 100 mm, 3μm	ESI/QQQ/MRM⁺	CP IF PCP	261/154.1 261/140.1 249/164.1	0.1 μg/L 0.1 μg/L	[25]
cyclophosphamide ifosphamide	SPE C18 ethylacetate	RP C8/gradient HCOOH/ACN/MeOH 4.6 × 100 mm, 5μm	ESI/QQQ/SRM⁺	CP IF TRP	261.0/140.2 261.0/92.0 323.3/92.0	0.02 μg/L 0.04 μg/L	[26]
cyclophosphamide ifosphamide	SPE C18 MeOH	RP C18/gradient HCOOH/ACN/MeOH 2.1 × 150 mm, 3μm	ESI⁺/Ion Trap	CP IF PSL	261/140 261/182 361/343	0.4 μg/L 0.4 μg/L	[27]
cyclophosphamide ifosphamide	LLE dichloromethane	RP C18/gradient HCO₂NH₄/ACN 2.1 × 100 mm, 5 μm	ESI/QQQ/MRM⁺	CP d₄-CP IF	261/140 264/140 261/92	0.01 μg/L 0.01 μg/L	[28]
cyclophosphamide 4-keto-CP ifosphamide	LLE ethylacetate	RP C18/gradient HCOOH/ACN 3.0 × 250 mm, 3.5μm	ESI/QQQ/MRM⁺	CP 4-keto-CP IF d₆-CP	261/140 267/140 275/106 261/154	0.1 μg/L 1.0 μg/L 0.05 μg/L	[29]
cyclophosphamide 4-keto-CP carboxy-CP DCL-CP	LLE MeOH	RP C8/gradient HCOOH/MeOH 3.0 × 100 mm, 5μm	ESI/QQQ/SRM⁺	CP 4-keto-CP carboxy-CP DCL-CP d₄-CP	261/140 275/221 293/221 199/171 265/145	5 μg/L 5 μg/L 30 μg/L 1 μg/L	[30]
bendamustine (BM) & phase I metabolites	SPE MeOH	RP C18/gradient HCO₂NH₄/MeOH 2.0 × 150 mm, 4μm	ESI/QQQ/MRM⁺	BM BM-IS metabolite 3 metabolite 4	358/228 372/338 374/186 344/354	0.5 μg/L 0.5 μg/L 0.4 μg/L	[31]
bendamustine phase I metabolite	SPE MeOH	Polar RP/gradient HCO₂NH₄/MeOH 2.0 × 150 mm, 4μm	ESI/QQQ/MRM⁺	dihydroxy-BM α-DLA	322/304 408/170	1 μg/L	[31]

Legend of abbreviations used in Table 1. LC/MS determination of nitrogen mustard antineoplastic drugs in urine

ACN: acetonitrile, CH₂Cl₂, DCL-CP: N-dechloroethyl-cyclophosphamide, α-DLA: α-dansyl-L-arginine, ESI: electrospray ionization, LLE: liquid-liquid extraction, MeOH: methanol, MRM: multiple reaction monitoring, PCP: phencyclidine, PSL: prednisolone, QQQ: triple quadrupole, RP: reversed phase, SPE: solid phase extraction, SRM: single reaction monitoring, TRP: trophosphamide