A validated UPLC–MS/MS method for biomonitoring the exposure to the fragrance 7-hydroxycitronellal

Contaminants of emerging concern in urine: a review of analytical methods for determining diisocyanates, benzotriazoles, benzothiazoles, 4-methylbenzylidene camphor, isothiazolinones, fragrances, and non-phthalate plasticizers

“…As validation parameters, linearity, specificity, recovery, precision, and accuracy were tested. Precision and accuracy were always limited to at least 20%, but more often more stringent margins were used such as 15% (Asimakopoulos et al 2013a ; Stoeckelhuber et al 2017 ) or even 10% (Bhandari et al 2019 ; Höllerer et al 2018b ; Schettgen et al 2017 ). Lépine et al assessed the method’s accuracy by comparing the results with the samples from an external quality control assessment, such as the German External Quality Assessment Scheme (G-EQUAS).…”

“…Dried and derivatized with 3-NPA in WA (80 °C, 30 min) UPLC: Waters Acquity UPLC I-Class Column: Waters Acquity BEH C18 (100 mm × 2.1 mm, 1.7 μm) Mobile phases: A (MeOH), B (5 mM ammonium acetate with 0.025% ammonium hydroxide, pH 9.2), flow 0.35 mL/min Gradient elution: 80% B, 0–4 min, 80–55% B, 4–10 min, 55–35% B, 10–11 min, 35–0% B, 11–11.1 min, 0% B, 11.1–13 min, 0–80% B, 13–13.1 min, 80% B, 13.1–15 min ESI(-)-MS2-MRM: Waters TQ-S Triple Quadrupole 0.42, 0.1, 0.36, 0.45, 0.39 Pluym et al ( 2016 ) 7-HC 7-HCA LLE: 1 mL urine deconjugated (37 °C, 3 h), acidified and extracted with DCM. Dried and derivatized with 3-NPA (80 °C, 30 min) UPLC: Waters Acquity UPLC I-Class Column: Waters Acquity BEH C18 (100 mm × 2.1 mm, 1.7 μm) Mobile phases: A (0.1% FA/W), B (0.1% FA/ACN), flow 0.5 mL/min Gradient elution: 80% A, 0–1 min, 80–20% a, 1–5 min, 20% A, 5–5.5 min, 20–80% A, 5.5–7 min ESI(-)-MS2-MRM: Waters TQ-S Triple Quadrupole 0.5 Stoeckelhuber et al ( 2017 ) Benzotriazoles and benzothiazoles 1H-BTR , 1OH-BTR, TTR, XTR, 5-Cl-1H-BTR, BTH, 2-OH-BTH, 2-MeS-BTH, 2-amino-BTH, 2-SH-BTH, 2-SCNMeS-BTH 1H-BTR , 1OH-BTR, TTR, XTR, 5-Cl-1H-BTR, BTH, 2-OH-BTH, 2-MeS-BTH, 2-amino-BTH, 2-SH-BTH, 2-SCNMeS-BTH SPE: 2 mL, deconjugation with β-glucuronidase (37 °C, 24 h), diluted, pH adjusted to 3, extracted on Oasis HLB 6 cc/200 mg with MeOH/ACN (1:1), dried and reconstituted in 200 μL MeOH/ACN (1:1) LLE: 600 μL extracted with 6 mL ACN/DCM (1:1), extract dried and reconstituted in 150 μL MeOH/ACN HPLC: Agilent 1100 HPLC Column: Zorbax SB aq (150 × 2.1 mm, 3,5 μm), Mobile phases: A (0.1% FA/W), B (ACN), flow 0.25 mL/min Gradient elution: 10–40% B, 4.5 min, 40–100% B, 11.5 min, 100% B, 6.1 min, 10% B, 7.1 min ESI(+)-MS2-MRM:Applied Biosystems triple quadrupole SPE: 0.50, 2.00, 0.20, 0.20, 0.50, 5.00, 2.50, 0.20, 0.20, 0.50 LLE: 1.70, 0.70, 0.70, 1.70, 0.70. 17.00, 3.50, 1.70, 0.70, 1.70 Asimakopoulos et al ( 2013a ) 1H-BTR , 1OH-BTR, TTR, XTR, 5-Cl-1H-BTR, BTH, 2-OH-BTH, 2-MeS-BTH, 2-amino-BTH, 2-SCNMeS-BTH 1H-BTR , 1OH-BTR, TTR, XTR, 5-Cl-1H-BTR, BTH, 2-OH-BTH, 2-MeS-BTH, 2-amino-BTH, 2-SCNMeS-BTH LLE: 1 mL deconjugated with β-glucuronidase (37 °C, 24 h), extracted with 3 mL MTBE/EA (5/1), dried and reconstituted in 200 μL ACN/W (6/4) UPLC: Dionex Ultimate 3000 UHPLC Column: Thermo Hypersil GOLD (100 × 2.1 mm, 1.9 μm) Mobile phases: A (0.01% FA/W), B (ACN), flow 0.25 mL/min Gradient elution: 10–83% B, 9.5 min, 83–100%, 100% B, 3 min, 10% B ESI(+)-MS2-MRM: Thermo Scientific TSQ Quantiva Triple Quadrupole 0.2, 11, 2, 7, 4, 9, 6, 11, 4, 14 Li et al ( 2017 ...…”

“…To determine lysmeral and 7-HC biomarkers of exposure, two UPLC-based methods using ESI-MRM detection are presented (Pluym et al 2016 ; Stoeckelhuber et al 2017 ). Separation was achieved on a 100-mm C18 analytical column with a binary-solvent mixture.…”

“…The method for the determination of 7-HCA included 0.1% formic acid (FA) in acetonitrile (ACN) and aqueous 0.1% FA. Both methods report low LOQs for the studied compounds (≤ 0.5 ng/mL); however, internal standards have to be custom synthesized (Pluym et al 2016 ; Stoeckelhuber et al 2017 ), which limits the possibilities for many laboratories.…”