Page 65 - Clinical-Medical Solution for Clinical Chemistry

Application No.C142$
News

Q Calibration Curves
Fig. 4 shows calibration curves of 6 compounds spiked into urine. Meldonium was included in the World Anti-Doping
Agency (WADA) Prohibited List on 1 January 2016, the guidance for meldonium in urine samples collected after 30
September 2016 applies normal results management to samples above a concentration of 100 ng/mL. In this method,
the urine calibration range between 1 to 200 ng/mL resulted in a linear response for all compounds with regression
coefficients r2 > 0.997.

Meldonium
Area ratio (×100) (×1,000) (×10,000) (×1,000,000)
7.5 7:147.20 > 58.25 (+) 7:147.20 > 58.25 (+) 1.00 7:147.20 > 58.25 (+)
7:147.20 > 59.25 (+) 7:147.20 > 59.25 (+) 7:147.20 > 59.25 (+)
2
r = 0.9988
2.5 7.5
0.75
5.0
2.0 5.0
0.50
1.5
2.5
2.5
1.0 0.25
0.0 0.0 0.00
0.5
1ʙ200 ng/mL 8.0 8.5 8.0 8.5 8.0 8.5
0.0
0.0 25.0 50.0 75.0 Conc. ratio 1 ng/mL 10 ng/mL 100 ng/mL
Synefrine Norfenefrine Etilefrine Oxilofrine Octopamine
Area (×100,000) Area (×1,000,000) Area (×1,000,000) Area (×1,000,000) Area (×1,000,000)
r = 0.9991 r = 0.9993 1.00 r = 0.9984 r = 0.9974 r = 0.9985
6.0 2 2 2 2.0 2 1.25 2
5.0 1.00 1.00
1.5
4.0 0.75 0.75
0.75
3.0 0.50 0.50 1.0
2.0 0.50
0.25 0.25 0.5
1.0 0.25
0.0 0.00 0.00 0.0 0.00
0.0 25.0 50.0 75.0 Conc. 0.0 25.0 50.0 75.0 Conc. 0.0 25.0 50.0 75.0 Conc. 0.0 25.0 50.0 75.0 Conc. 0.0 25.0 50.0 75.0 Conc.
2ʙ200 ng/mL 2ʙ200 ng/mL 1ʙ200 ng/mL 1ʙ200 ng/mL 2ʙ200 ng/mL
Fig. 4 Calibration Curves and MRM Chromatograms of 6 Compounds
Q Analysis of Synephrine, Etilefrine and Oxilofrineine in Urine
(DFK XULQH VDPSOHV ZHUH FROOHFWHG IURP YROXQWHHUV EHLQJ VHSDUDWHO\ DGPLQLVWHUHG ZLWK V\QHSKULQH HWLOHIULQH DQG R[LORIULQH
ZHUH DQDO\]HG XVLQJ ' +,/,& 6\VWHP. ,Q DOO VDPSOHV ERWK WKH XQFKDQJHG IRUP DQG VXOSKDWHG PHWDEROLWHV ZHUH GHWHFWHG
Unchanged form Sulphate (Positive ion) Sulphate (Negative ion)
(×10,000) (×1,000,000) (×1,000,000)
5.0 6:168.20 > 135.20 (+) 1.50 3:248.20 > 150.25 (+) 14:246.20 > 148.20 (-)
6:168.20 > 107.25 (+) 3:248.20 > 135.20 (+) 5.0 14:246.20 > 106.10 (-)
4.0 1.25 4.0
Urine: Synephrine-administered 97.24 ng/mL 1.00
3.0 3.0
(×10 dilution) 0.75
2.0 2.0
0.50
1.0 0.25 1.0
0.0 0.00 0.0
5.50 5.75 6.00 6.25 5.25 5.50 5.75 6.00 5.25 5.50 5.75 6.00
(×10,000) (×100,000) (×1,000,000)
4.0
4:182.30 > 135.25 (+) 1:262.20 > 164.15 (+) 11:260.20 > 180.20 (-)
4:182.30 > 91.25 (+) 2.0 11:260.20 > 121.10 (-)
4.0
3.0
Urine: Etilefrine-administered 27.71 ng/mL 3.0 1.5
(×10 dilution) 2.0
2.0 1.0
1.0 1.0 0.5
0.0 0.0 0.0
5.00 5.25 5.50 5.75 4.75 5.00 5.25 5.50 4.75 5.00 5.25 5.50
(×10,000) (×1,000)
5:182.30 > 149.25 (+) 12:260.20 > 77.10 (-)
5:182.30 > 105.25 (+) 12:260.20 > 178.20 (-)
2.0 4.0
Urine: Oxilofrine-administered 1.5 1.159 ng/mL 3.0
1.0 2.0
0.5 1.0
0.0 0.0
5.25 5.50 5.75 6.00 5.00 5.25 5.50 5.75
Fig. 5 Results of Urine: Synephrine, Etilefrine and Oxilofrine were separately administered