Liquid chromatography-tandem mass spectrometry for the identification of impurities in d-allethrin samples.
A previous GC/MS study highlighting the impurity profile of the synthetic pesticide d-allethrin is extended here to validate and confirm the impurities identity through the development of soft ionisation HPLC-MS methods. To accomplish this, we developed a reverse phase LC-MS analysis in gradient elution with two distinct soft ionisation techniques, the atmospheric pressure ionisation with electrospray source (API-ESI) and the chemical ionisation (APCI). A single quadrupole and an ion trap, which allowed the simultaneous determination of the molecular masses and structural information of the impurities by acquisition of collisionally induced (CID) product ions spectrum and in-source fragmentation, were employed as analysers. Single quadrupole and ion trap analysers resulted perfectly matching in the d-allethrin impurity fragmentation patterns. All the main impurities over 0.1% identified by GC/MS were confirmed. Results indicate that the proposed HPLC/MS method was found appropriate to confirm the presence of impurities such as chrysolactone, chloro allethrin derivatives, allethrolone and chrysanthemic acid, excluding their formation under GC/MS strong ionisation condition.
Fiori
J
J
Dip. Scienze Farmaceutiche, Via Belmeloro 6, 40126 Bologna, Italy.
Bragieri
M
M
Zanotti
M C
MC
Liverani
A
A
Borzatta
V
V
Mancini
F
F
Cavrini
V
V
Andrisano
V
V
D000487:Allethrins / Q000031:analogs & derivatives* / Q000737:chemistry*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D008962:Models, Theoretical; D010575:Pesticides / Q000737:chemistry*; D013056:Spectrophotometry, Ultraviolet; D013237:Stereoisomerism
D000487:Allethrins; D010575:Pesticides