| GHRPs and GHSs |
WADA ISO/IEC 17025 |
RP-HPLC, Kinetex C18 column (100
mm × 2.1 mm, 2.6 μm),
mobile phase A (0.1% FA in water), B (0.1% FA in ACN), temperature
oven 35 °C, flow rate 0.5 mL/min; 5/95/95/5/5% B in 0.5/5.5/6.5/8.0 min; LC–MS/MS
conditions: ESI-triple quadrupole, ion spray voltages: 4.5 kV in positive
mode; capillary and vaporizer temperatures: 320 °C, sheath and auxiliary gas flow rate: 60 arbitrary units, respectively97
|
matrix: urine; pretreatment sample: IE/RP-SPE97
|
| mixture of peptides used in doping |
ISO-17025 |
RP-HPLC, ACQUITY UPLC CSH
C18 column (100 × 1 mm2, 1.7 μm), 210 nm, mobile
phase A (0.1% FA in water), B (0.1%
FA in ACN), temperature oven: 35 °C, flow rate: 0.3 mL/min; 2/2/24/30/50/99/99/2/2% B in 1/2/13/21/23/24/26/27/32 min; screening: UPLC-DAD, ESI-IT, mode positive, spray
voltage: 4.5 kV, end plate voltage: 500 V; nebulizer 2 bar, desolvation
gas temperature: 250 °C at a flow rate: 10 L/min101
|
matrix: water;
pretreatment sample: centrifugation101
|
| mixture of peptides
used in doping |
WADA |
UHPLC, HF-X Hybrid
Quadrupole-Orbitrap, A Poroshell 120 EC-C8
analytical column (3 × 50 mm, 2.7 μm), mobile phase A (0.1% FA in water), B (0.1% FA, 1% DMSO in
ACN), temperature column: 30 °C, flow rate: 0.35 mL/min; 1/40/90/90/1% B in 1/11/11.5/13/16 min; mode positive, ionization voltage: 3.3 kV90
|
matrix: blood pretreatment sample: centrifugation90
|
| mixture of peptides used in doping |
WADA-ISO/IEC 17025 |
UHPLC, Agilent Poroshell 120 ECC18 column (50 × 2.1 mm,
2.7 μm), mobile phase A (0.2% FA in water), B (0.2% FA in ACN),
temperature column: 40 °C, flow
rate 0.4 mL/min; 1/1/60/100/1/1% B in 0/1/7/7.1/9.1/9.2/11 min; injection volume: 10 μL, Q-TOF parameters: positive mode,
drying and nebulizing gas: nitrogen; drying gas flow: 12 L/min, 250 °C, nebulizer gas pressure: 40 psi, sheath gas flow: 8 L/min, 350 °C; capillary and nozzle voltages were 4000 and 1000 V, respectively55
|
matrix: urine; pretreatment sample: RP-SPE55
|
| GHRHs |
N.R. |
UHPLC, Waters Symmetry trapping column C18
(180 μm ×
20 mm, 5 μm), mobile phase A (0.1% FA in water), B (0.1% FA
in ACN), flow rate: 350 nL/min; 1/60/80/1/1% B in 0/20/22/23/31 min; Q-Orbitrap parameters: positive mode, transfer capillary temperature:
150 °C, spray voltage: 2 kV102
|
matrix: plasma; pretreatment sample: immunoaffinity-SPE102
|
| GHRP-6 |
FDA |
Nano-HPLC-Q-TOF, monolithic nanocolumn
(200 μm ×
5 cm) and a trap column (200 μm × 5 mm) from LC Packings,
mobile phase A (0.1% FA in water), B (0.1% FA in ACN/water 80/20 v/v), flow rate: 0.8 μL/min; 50/100/100/10% B in 0/2/5/7 min; capillary voltage: 2.5 kV; cone voltage: 40 V103
|
matrix: human
plasma; pretreatment sample: precipitation, centrifugation,
and desalting103
|
| IGF-1 |
WADA-ISO/IEC 17025 |
UHPLC-Q-Exactive, Kinetex
C18 column (100 × 2.1 mm, 2.6
μm), mobile phase A (0.1% FA in water), B (0.1% FA in MeOH),
temperature column: 40 °C, flow
rate: 300 μL/min; gradient elution 2/2/95/5/5% B in 0/0.5/8.5/10/12.5 min, mode positive, ion spray voltage: 4.5 kV, capillary
heaters temperature: 320 °C, probe
heaters: 438 °C, sheath gas flow
rate: 51 arbitrary units, auxiliary gas flow rate: 14 arbitrary units98
|
matrix: mouse serum; pretreatment
sample: trypsin digestion, IS 15N-IGF-I98
|
| Leuprolide |
ICH |
HPLC, HILIC column (150 mm × 2.1 mm,
6 μm), mobile
phase [25 mL CH3COONH4 (0.2 M), 320 mL acetic
acid (0.522 M) pH 3], 655 mL water/ACN with 1% FA 25/75, v/v, isocratic elution, flow rate: 1.0 mL/min, temperature column: 25 °C; API-triple
quadrupole, mode positive; sheath, auxiliary, and ion sweep gas: nitrogen;
ion spray voltage: 5.5 kV, capillary temperature: 750 °C100
|
matrix: human plasma or serum; pretreatment sample: RP-SPE100
|
| desmopressin and vasopressin |
N.R. |
RP-HPLC, Pyramid C18 column (50 mm × 2.1 mm, 1.9 μm),
mobile phase A (0.1% FA in water), B (ACN), gradient elution: 0/100/100/0/0% B, in 0/8/8.5/9/15 min; flow rate: 0.3 mL/min triple quadrupole-TOF, mode positive at 500 °C; collision and auxiliary/sheath gas nitrogen104
|
matrix: urine; pretreatment sample: EI-RP-SPE104
|
