Page 58 - Clinical-Medical Solution for Clinical Chemistry

A Novel Platform of On-line Sample Pre-treatment and LC/MS/MS
Analysis for Screening and Quantitation of Illicit Drugs in Urine

Results and Discussion

MRM-based method for eighteen illicit drugs

Table 2 shows the summarized results of optimized MRM with one as the quantitation ion and the other two for
transitions and parameters of the eighteen analytes and con rmation. A gradient elution program was optimized
fourteen isotope-labelled internal standards (IS). However, with a total runtime of eleven minutes. The MRM
four isotope-labelled ISs were not available. Three MRM chromatograms of a mixed standard sample in urine are
transitions were selected for each compound except PROP shown in Figure 3.

(x100,000) (x100,000) (x100,000)
2.0 (x10,000)
2:296.10>250.20(+) 3.0 4:238.10>125.15(+) 5:224.10>125.15(+) 4.0 13:468.30>55.15(+)
2:296.10>221.20(+) 4:238.10>220.20(+) 5:224.10>207.15(+) 13:468.30>396.30(+)
1.5 2:296.10>165.15(+) Nimetazepam NIME 4:238.10>207.15(+) Ketamine KET 2.0 5:224.10>179.20(+) Norketamine NORKET 3.0 13:468.30>414.35(+) Buprenorphine BU
1.0 2.0
2.0
1.0
0.5 1.0 1.0
0.0 0.0 0.0 0.0
5.0 6.0 7.0 8.0 3.0 4.0 5.0 6.0 3.0 4.0 5.0 6.0 4.0 5.0 6.0 7.0
(x10,000) (x1,000) (x10,000) (x10,000)
2.0 14:414.20>101.10(+) 17:286.10>200.90(+) 3.0 18:300.10>164.85(+) 20:328.10>164.90(+)
14:414.20>83.20(+) NORBU 17:286.10>151.85(+) MORP 18:300.10>214.90(+) Codeine COD 20:328.10>210.90(+) MAM 6-MAM
1.5 14:414.20>187.20(+) Norbuprenorphine 5.0 17:286.10>164.90(+) Morphine 2.0 18:300.10>151.80(+) 5.0 20:328.10>192.85(+)
1.0
2.5 1.0 2.5
0.5
0.0 0.0 0.0 0.0
3.0 4.0 5.0 6.0 1.0 2.0 3.0 4.0 2.0 3.0 4.0 5.0 2.0 3.0 4.0 5.0
(x100,000) (x1,000,000) (x100,000) (x1,000,000)
2.0 23:290.20>168.20(+) 24:244.30>86.20(+) 25:251.20>132.15(+) 26:310.20>265.25(+)
23:290.20>105.10(+) BE 1.00 24:244.30>159.25(+) PCP 4.0 25:251.20>91.15(+) METQ 26:310.20>105.10(+) METD
23:290.20>77.10(+) 24:244.30>91.15(+) 25:251.20>65.20(+) 1.0 26:310.20>77.10(+) Methadone
1.5 0.75 Phencyclidine (PCP) 3.0 Methaqualone
1.0 Benzoylecgonine (BE) 0.50 2.0 0.5
0.5 0.25 1.0
0.0 0.00 0.0 0.0
3.0 4.0 5.0 6.0 4.0 5.0 6.0 7.0 4.0 5.0 6.0 7.0 4.0 5.0 6.0 7.0
(x100,000) (x100,000) (x100,000) (x100,000)
30:194.20>163.25(+)
27:136.30>91.05(+) 28:208.30>163.20(+) 29:180.30>163.20(+) MDA MDMA
2.0 27:136.30>119.10(+) AMPH 3.0 28:208.30>105.15(+) MDEA MDEA 29:180.30>135.15(+) MDA 4.0 30:194.20>105.20(+) MDMA
30:194.20>133.20(+)
27:136.30>65.00(+) Amphetamine 28:208.30>135.10(+) 1.0 29:180.30>79.20(+)
1.5 2.0 3.0
2.0
1.0 0.5
1.0 1.0
0.5
0.0 0.0 0.0 0.0
2.0 3.0 4.0 5.0 2.0 3.0 4.0 5.0 2.0 3.0 4.0 5.0 2.0 3.0 4.0 5.0
(x100,000) (x100,000)
7.5 31:340.20>58.15(+) 32:150.30>91.15(+)
Propoxyphene 32:150.30>119.20(+)
31:340.20>266.30(+) PROP 3.0 32:150.30>65.10(+) METH
5.0 2.0 Methamphetamine
2.5 1.0
0.0 0.0
4.0 5.0 6.0 7.0 2.0 3.0 4.0 5.0
Figure 3: Individual MRM chromatograms of eighteen illicit drugs each (200 ng/mL) and
fourteen ISs (100 ng/mL) spiked in urine obtained on CLAM-LC/MS/MS platform.

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