Table I.
Method Validation Results for Working Surfaces and Urine Samples
| Analyte | |||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Surface samples | Parameter | CPa | GEMa | DACAa | IRIb | MTXb | ETPb | DOCEa | VBNb | PACLIc | DOXOLc | DOXOc | EPIc |
| Linearity (pg/cm2) | 5–5,000 | 10–5,000 | 50–5,000 | 50–5,000 | 50–5,000 | 50–5,000 | 50–5,000 | 100–5,000 | – | – | – | – | |
| LOD (pg/cm2) | 5 | 5 | 5 | 5 | 5 | 50 | 50 | 100 | 50 | 50 | 100 | 100 | |
| LOQ (pg/cm2) | 5 | 10 | 50 | 50 | 50 | 50 | 100 | 100 | – | – | – | – | |
| Inaccuracy (MRE) | –0.9 to 0.0 | –2.0 to 8.4 | –4.4 to 2.6 | –10.3 to −7.5 | 5.3–6.5 | –11.0 to 1.4 | 2.9–12.5 | 1.7–4.3 | – | – | – | – | |
| Imprecision (%CV) | 5.2–11.3 | 9.9–11.4 | 8.6–9.1 | 16.1–20.1 | 11.7–13.5 | 15.1–22.1 | 10.0–13.7 | 13.4–15.3 | – | – | – | – | |
| Interference studies | No interferences | ||||||||||||
| Matrix effectd | –58.3 to 1,268.9% | ||||||||||||
| Extraction efficiencyd | 10.8–75% | ||||||||||||
| Process efficiencyd | 15.5–683.9% | ||||||||||||
| Autosampler stability | –4.2 to 4.5 | –3.1 to 0.0 | –1.9 to 2.4 | 2.9–3.2 | –1.5 to −0.7 | –1.1 to 1.1 | –18.7 to −0.3 | –3.0 to 8.6 | – | – | – | – | |
| Freezer stability | –2.3 to −0.9 | –12.0 to −4.4 | 0.3–2.0 | 0.2–1.8 | –2.9 to −2.0 | –0.4 to 0.0 | –1.8 to 10.6 | –9.5 to 6.6 | – | – | – | – | |
| Analyte | |||||||||||||
| Urine samples | Parameter | CPa | GEMa | DACAa | IRIa | MTXa | DOCEa | VBNa | PACLIa | DOXOc | DOXOLa | EPIc | |
| Linearity (pg/mL) | 20–1,000 | 250–5,000 | 50–1,000 | 10–1,000 | 10–1,000 | 100–5,000 | 10–1,000 | 10–1,000 | – | 10–1,000 | – | ||
| LOD (pg/mL) | 20 | 250 | 50 | 5 | 5 | 100 | 10 | 5 | 50 | 10 | 10 | ||
| LOQ (pg/mL) | 20 | 250 | 50 | 10 | 10 | 100 | 10 | 10 | – | – | – | ||
| Inaccuracy (MRE) | –3.7 to −0.5 | –3.8 to 0.7 | 2.4–4.4 | –2.5 to 2.0 | –4.1 to −3.4 | –0.7 to 14.9 | 0.3–2.5 | –3.6 to 0.3 | – | –1.9 to 2.2 | – | ||
| Imprecision (%CV) | 4.3–5.9 | 11.2–12.4 | 3.9–5.1 | 3.7–6.2 | 5.5–9.6 | 2.9–9.5 | 3.7–8.3 | 2.6–7.1 | – | 6.6–7.5 | – | ||
| Interference studies | No interferences | ||||||||||||
| Matrix effectd | –66.7% to 1,636.0% | ||||||||||||
| Extraction efficiencyd | 47.1–130.4% | ||||||||||||
| Process efficiencyd | 28.5–1,438.8% | ||||||||||||
| Autosampler stability | –0.8 to 3.1 | 8.9–9.5 | –1.9 to 1.3 | –4.0 to −2.8 | 2.4–2.7 | –12.7 to −1.9 | –11.3 to 2.0 | 0.2–2.1 | – | –4.1 to 1.6 | – | ||
| Freezer stability | –9.1 to −3.7 | 4.0–12.7 | –10.2 to −8.6 | 1.5–7.2 | –2.0 to 6.4 | 7.4–8.8 | –3.1 to 12.2 | –8.7 to −0.9 | – | –0.5 to 4.4 | – | ||
| Freeze/thaw stability | 7.7–16.0 | 2.8–11.7 | –19.8 to −19.0 | –12.5 to −1.7 | –6.0 to −5.8 | –9.6 to 2.1 | –0.2 to 6.0 | –6.4 to −13.3 | – | –13.1 to −11.3 | – | ||
CP: cyclophosphamide, CV: coefficient of variation; DACA: dacarbazine; DOCE: docetaxel; DOXO: doxorubicin; DOXOL: doxorubicinol; EPI: epirubicin; ETP: etoposide; GEM: gemcitabine; IRI: irinotecan; MRE: mean relative error; MTX: methotrexate; PACLI: paclitaxel; VBN: vinorelbine.
a
Linear regression and 1/x weighting factor;
b
Quadratic regression and 1/x weighting factor;
c
Qualitatively validated compounds;
d
Specific ranges for each analyte are displayed in the Supplemental material (Tables S3 and S4).