US 12,340,996 B2
Method for rapid on-site detection of fentanyl analogs using a miniature mass spectrometer
Qiang Ma, Beijing (CN); Xiangyu Guo, Beijing (CN); Hua Bai, Beijing (CN); and Wentao Li, Beijing (CN)
Assigned to Chinese Academy of Inspection and Quarantine, Beijing (CN)
Filed by Chinese Academy of Inspection and Quarantine, Beijing (CN)
Filed on Sep. 9, 2022, as Appl. No. 17/941,095.
Application 17/941,095 is a continuation of application No. PCT/CN2021/079645, filed on Mar. 9, 2021.
Claims priority of application No. 202010181694.9 (CN), filed on Mar. 16, 2020.
Prior Publication US 2023/0015987 A1, Jan. 19, 2023
Int. Cl. H01J 49/00 (2006.01)
CPC H01J 49/0013 (2013.01) [H01J 49/0031 (2013.01)] 4 Claims
OG exemplary drawing
 
1. A method for rapid on-site detection of fentanyl analogs using a miniature mass spectrometer, comprising the following steps:
(1) selecting a spotting plate;
(2) loading a sample: depositing the sample and 3-nitrobenzonitrile solution in acetonitrile on the spotting plate to form a crystalline mixture;
(3) carrying out analysis and detection: setting the parameters of the miniature mass spectrometer, placing the crystalline mixture on the spotting plate in close proximity to the inlet of the miniature mass spectrometer, and facilitating the ionization of the crystalline mixture for the analysis and detection of fentanyl analogs;
wherein the sample comprises powder, blood, and sweat; there are 49 kinds of fentanyl analogs, and the analysis parameters of the miniature mass spectrometer and LODs in step (3) are as shown in Table 1;
TABLE 1
 
The analysis parameters of the miniature mass spectrometer and limits of detection(LODs) for the 49 fentanyl analogs
 
 Ionization
 
 
 
 
 
 
Fentanyl analogs mode m/z RF/kHz AC/kHz CID-AC/kHz CID-AC/Vpp LOD/(μg/kg)
 
fentanyl positive 337 150-800 5-46 47 220 20
para-flufentanyl positive 355 150-880 5-42 43 220 20
meta-flufentanyl positive 355 150-860 5-43 44 220 20
ortho-flufentanyl positive 355 150-860 5-42 43 210 20
N-phenyl-N-[1-[2-(2-thienyl)ethyl]- positive 343 150-840 5-44 45 220 50
4-piperidyl]propanamide
acetylfentanyl positive 323 150-780 5-45 46 210 50
N-(2-fluorophenyl)-N-(1- positive 341 150-820 5-44 45 215 20
phenethylpiperidin-4-yl)acetamide
N-(3-fluorophenyl)-N-(1- positive 341 150-820 5-44 45 220 20
phenethylpiperidin-4-yl)acetamide
N-(4-fluorophenyl)-N-[1-(2- positive 341 150-820 5-44 45 220 20
phenylethyl)-4-piperidinyl]-
acetamide
butyrfentanyl positive 351 150-830 5-43 44 235 50
isobutyryl fentanyl positive 351 150-840 5-42 43 222 50
4-fluorobutyrfentanyl positive 369 150-900 5-40 41 225 50
meta-fluorobutyryl fentanyl positive 369 150-880 5-40 41 220 50
N-(2-fluorophenyl)-N-(1- positive 369 150-880 5-40 41 220 50
phenethylpiperidin-4-yl)butyramide
para-fluoroisobutyrfentanyl positive 369 150-880 5-40 41 220 50
cis-3-methylfentanyl positive 351 150-850 5-43 44 223 50
trans-3-methylfentanyl positive 351 150-850 5-43 44 221 50
alpha-methylfentanyl positive 351 150-850 5-43 44 220 50
N-[1-[1-methyl-2-(2-thienyl)ethyl]-4- positive 357 150-870 5-42 43 217 100
piperidyl]-N-phenylpropanamide
cis-3-methylthiofentanyl positive 357 150-880 5-42 43 215 100
2-methoxy-N-phenyl-N-[1-(2- positive 353 150-840 5-43 44 210 20
phenylethyl)-4-piperidinyl]-
acetamide
para-methoxy acetyl fentanyl positive 353 150-840 5-42 43 220 20
N-(2-fluorophenyl)-N-(1- positive 353 150-820 5-43 44 215 20
phenethylpiperidin-4-yl)acrylamide
N-[1-(2-hydroxy-2-phenylethyl)-4- positive 353 150-840 5-42 43 220 200
piperidyl]-N-phenylpropanamide
norfentanyl positive 232 150-600 5-67 68 180 50
acrylfentanyl positive 335 150-820 5-44 45 220 50
methyl-4-(N-phenylpropionamido)- positive 395 150-930 5-36 37 200 100
1-phenethylpiperidine-4-carboxylate
furanylfentanyl positive 375 150-920 5-40 41 205 50
valerylfentanyl positive 365 150-900 5-40 41 225 50
ocfentanil positive 371 150-880 5-40 41 215 50
remifentanil positive 377 150-940 5-39 40 180 200
sufentanyl positive 387 150-950 5-37 38 190 100
alfentanil positive 417  150-1000 5-34 35 200 200
N-phenyl-N-(1-phenethylpiperidin-4- positive 379 150-940 5-38 39 205 50
yl)tetrahydrofuran-2-carboxamide
heptanoyl fentanyl positive 394 150-920 5-36 37 225 50
phenyl fentanyl positive 385 150-950 5-38 39 210 20
hexanoyl fentanyl positive 380 150-940 5-38 39 230 50
N-phenyl-N-(1-(2-(thiophen-2- positive 329 150-800 5-45 46 215 100
yl)ethyl)piperidin-4-yl)acetamide
N-(1-(2-hydroxy-2-(thiophen-2- positive 359 150-890 5-41 42 213 200
yl)ethyl)piperidin-4-yl)-N-
phenylpropanamide
meta-fluoro methoxyacetyl fentanyl positive 371 150-890 5-40 41 200 50
acetyl-alpha-methylfentanyl positive 337 150-800 5-44 45 226 20
para-methoxy methoxyacetyl positive 383 150-910 5-38 39 210 50
fentanyl
beta-hydroxy-3-methylfentanyl positive 367 150-900 5-40 41 225 50
para-methoxy acryl fentanyl positive 365 150-900 5-40 41 220 50
para-methoxy tetrahydrofuran positive 409 150-920 5-35 36 210 20
cyclopentyl fentanyl positive 378 150-890 5-39 40 210 50
thiophene fentanyl positive 392 150-920 5-37 38 210 50
1-phenethyl-4-piperidone positive 204 150-500 5-76 77 220 20
1-phenethyl-N-phenylpiperidin-4- positive 281 150-670 5-55 56 230 20
amine
 
wherein the spotting plate is a triangular paper substrate.