US 2021/0063375 A1 · SCREENING AND CONFIRMATION METHOD FOR VETERINARY DRUGS AND ADDITIVES IN ANIMAL-DERIVED FOOD

Abstract

A screening and confirmation method for veterinary drugs and additives in animal-derived food, including: preparation of standard working solution, pretreatment of samples to be tested, establishment of database, sample detection, compound screening and compound confirmation. The disclosure employs ultra high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry, and enables the simultaneous detection of 207 veterinary drugs and additives in animal-derived food within 22 min.

A screening and confirmation method for veterinary drugs and additives in animal-derived food, comprising:

(1) dissolving 10 mg of each reference standard of the veterinary drugs and additives followed by diluting to 10 mL in a volumetric flask to prepare a 1 mg/mL stock solution of each reference standard;
wherein the veterinary drugs and additives are selected from:
(a) sulfonamides:
sulfamethazine, sulformethoxine, sulfisoxazole, sulfaguanidine, sulfamerazine, sulfamethylthiadizaole, sulfamethoxazole, sulfamethoxydiazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfamethazole, sulfapyridinee, sulfaquinoxaline, sulfathiazole, sulfisomidine, trimethoprim, diaveridine, phthalylsulfathiazole, sulfabenzamide, sulfacetamide, sulfachlorpyridazine, sulfachloropyrazine, sulfadiazine and sulfadimethoxine;
(b) fluoroquinolones:
lomefloxacin, marbofloxacin, nadifloxacin, nalidixic acid, norfloxacin, ofloxacin, orbifloxacin, oxolinic acid, pipemidic acid, pefloxacin, cinoxacin, sarafloxacin, sparfloxacin, ciprofloxacin, danofloxacin, difloxacin, enoxacin, enrofloxacin, fleroxacin, flumequine and gatifloxacin;
(c) benzimidazoles:
mebendazole, mebendazole-amine, 2-aminofluorobenzimidazole, oxfendazole, oxibendazole, parbendazole, 5-hydroxythiabendazole, tiabendazole, albendazole, albendazole sulfone, albendazole sulfoxide, amino albendazole sulfone, benzimidazole, febantel and lobendazole;
(d) stimulants:
cyproheptadine, fenoterol, labetalol, penbutolol, phenylethanolamine A, ractopamine, salbutamol, salmeterol, terbutaline, mabuterol, tulobuterol, bambuterol, brombuterol, cimaterol, cimbuterol, clenbuterol, clenproperol and clonidine;
(e) hormones:
chlormadinone acetate, 17a-methyltestosterone, clobetasol propionate, clobetasone butyrate, corticosterone, hydrocortisone, cortisone acetate, cortisone, deflazacort, dexamethasone, diflorasone diacetate, epitestosterone, estradiol benzoate, fludrocortisone acetate, flumetasone pivalate, flumethasone, fluocinolone acetonide, fluorometholone, flurandrenolide, fluticasone propionate, nandrolone propionate, halcinonide, dihydrodiethylstilbestrol, medroxyprogesterone acetate, megestrol acetate, melengestrol acetate, methandienone, methylprednisolone, norethindrone, nandrolone propionate, levonorgestrel, prednicarbate, prednisolone, prednisone, progesterone, dehydrotestosterone, testosterone, trenbolone, triamcinolone acetonide, beclomethasone, betamethasone dipropionate, betamethasone valerate and betamethasone;
(f) nitroimidazoles:
dimetridazole, ipronidazole, metronidazole, ornidazole, hydroxydimetridazole, ronidazole, secnidazole and tinidazole;
(g) antiviral drugs:
amantadine and rimantadine;
(h) lincosamide:
clindamycin and lincomycin;
(i) amphenicols:
chloramphenicol, florfenicol and thiamphenicol;
(j) penicillins:
ceftiofur, flucloxacillin, cloxacillin, nafcillin, piperacillin and penicillin G;
(k) quinoxalines:
quinocetone;
(l) antipyretics and analgesics:
phenacetin, salicylic acid, amidopyrine, antipyrine, dapsone, flunixin meglumine and acetaminophen;
(m) psychoactive drugs:
haloperidol, imipramine, nitrazepam, oxazepam, pemoline, perphenazine, promethazine, propionylpromazine hydrochloride, sulpiride, xylazine, acepromazin, anisopirol, azaperone, carbamazepine, chloropromazine, diazepam, diphenhydramine, droperidol, estazolam, clarithromycin, tiamulin, erythromycin, kitasamycin, tilmicosin and tylosin;
(n) anthelmintics:
toltrazuril sulfoxide, clopidol, dinitolmide, halofuginone and levamisole;
(o) pesticides:
buprofezin, carboxin, 3-hydroxycarbofuran, clothianidin, cyromazine, diuron, ethopabate, fipronil, fluridone, acephate, hexazinone, imazalil, imidacloprid, linuron, metribuzin, myclobutanil, acetamiprid, norflurazon, propyzamide, atrazine, simazine, desethyl atrazine, azoxystrobin and benoxacor;
(p) other substances:
scopolamine, valnemulin and atropine;
the norfloxacin is dissolved with water and diluted with methanol to 10 mL;
each of the pesticides is dissolved with acetone and then diluted with methanol to 10 mL;
each of the diaveridine, albendazole, albendazole sulfone and febantel is dissolved with formic acid and diluted with methanol to 10 mL;
and the rest substances are dissolved with a mixed solvent of methanol and ammonia water or a mixed solvent of methanol and dimethyl sulfoxide, and then diluted with methanol to 10 mL;
(2) pipetting 100 μL of the stock solution of each reference standard in the same category in Table 1 to a volumetric flask followed by diluting with methanol to 10 mL to accordingly prepare 16 first mixed standard solutions, wherein a concentration of each reference standard in the corresponding first mixed standard solution thereof is 10 μg/mL;
pipetting 100 μL of each first mixed standard solution to another volumetric flask followed by diluting with methanol to 10 mL to prepare a second mixed standard solution, wherein each reference standard in the second mixed standard solution has a concentration of 100 ng/mL;
and pipetting 100 μL, 500 μL, 1 mL and 5 mL, respectively, to a volumetric flask followed by diluting with a 20% aqueous methanol solution to 10 mL to prepare a series of mixed standard working solutions, wherein each reference standard in the series of mixed standard working solutions has a concentration of 1 ng/mL, 5 ng/mL, 10 ng/mL and 50 ng/mL, respectively;
(3) adding 5 g of a sample to a 50 mL centrifuge tube;
adding an extracting solution followed by vortex mixing;
shaking and centrifuging the centrifuge tube;
transferring a first supernatant to another 50 mL centrifuge tube;
if the sample is muscle or poultry egg, treating a precipitate with the extracting solution again to collect an extract;
combining the first supernatant with the extract to produce a mixture;
adding 6 g of anhydrous sodium sulfate and 1.5 g of sodium chloride to the mixture followed by vortex mixing for 30 s and standing;
and centrifuging the another 50 mL centrifuge tube to produce a second supernatant;
if the sample is cow's milk or goat's milk, adding 4 g of anhydrous sodium sulfate and 1 g of sodium chloride to the first supernatant followed by vortex mixing for 30 s and standing;
and centrifuging the another 50 mL centrifuge tube to produce a second supernatant;
(4) activating and equilibrating a solid phase extraction column sequentially with 4 mL of methanol and 4 mL of water;
rinsing the solid phase extraction column with 2 mL of the second supernatant and discarding a first effluent;
loading 5 mL of the second supernatant to the solid phase extraction column and collecting a second effluent with a centrifuge tube;
drying 4 mL of the second effluent in nitrogen flow at 40° C.;
adding 200 μL of methanol to the dried product followed by vortex mixing for 10 s;
adding 800 μL of pure water followed by vortex mixing for 30 s to produce a sample solution;
and filtering the sample solution with 0.22 m nylon filter membrane and collecting a filtrate for use;
(5) diluting each of the first mixed standard solutions such that each reference standard in the corresponding diluted first mixed standard solution thereof has a concentration of 1 μg/mL;
subjecting each of the diluted first mixed standard solutions to full scan and secondary scan in positive and negative modes using a ultra high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometer;
analyzing the scan results to obtain information of each reference standard through Trace Finder software of Q-Exactive plus;
and establishing a mass spectrometry database based on the information of each reference standard;
wherein the information of each reference standard comprises retention time, precise molecular weight of parent ion, addition mode, fragment ions, isotope abundance ratio and a fragment ion mass spectrometry generated through the superposition of fragment ion mass spectrometry obtained at collision energies of 20 eV, 40 eV and 60 eV;
the isomeride are further identified through the analysis of single standard reference;
and the mass spectrometry database is shown in Table 1;
TABLE 1
Mass spectrometry library information
Retention
Molecular
Addition
Parent
time
Category
Compound
formula
mode
ion
Fragment 1
Fragment 2
(min)
Sulfonamides
Sulfamethazine
C12H14N4O2S
M + H
279.09102
156.01138
124.08694
8.44
Sulformethoxine
C12H14N4O4S
M + H
311.08085
156.01138
140.04545
9.55
Sulfisoxazole
C11H13N3O3S
M + H
268.07504
156.0111
108.04462
9.83
Sulfaguanidine
C7H10N4O2S
M + H
215.05972
156.01138
108.04439
3.43
Sulfamerazine
C11H12N4O2S
M + H
265.07537
190.02809
156.01138
7.89
Sulfamethylthiadizaole
C9H10N4O2S2
M + H
271.03179
156.01138
108.04439
8.31
Sulfamethoxazole
C10H11N3O3S
M + H
254.05939
156.01138
108.04439
9.57
Sulfamethoxydiazine
C11H12N4O3S
M + H
281.07029
108.04465
156.01115
8.53
Sulfamethoxypyridazine
C11H12N4O3S
M + H
281.07029
215.09274
156.01138
8.41
Sulfamonomethoxine
C11H12N4O3S
M + H
281.07029
215.09274
156.01138
8.9
Sulfamethazole
C11H13N3O3S
M + H
268.07504
156.0111
108.04462
8.03
Sulfapyridinee
C11H11N3O2S
M + H
250.06447
184.08692
156.01138
7.55
Sulfaquinoxaline
C14H12N4O2S
M + H
301.07537
156.01138
108.04439
10.39
Sulfathiazole
C9H9N3O2S2
M + H
256.02089
156.01138
108.04439
7.28
Sulfisomidine
C12H14N4O2S
M + H
279.09102
124.08692
108.04439
6.57
Trimethoprim
C14H1SN4O3
M + H
291.14517
275.11387
261.09822
7.28
Diaveridine
C13H16N4O2
M + H
261.1346
245.1033
123.06652
7
Phthalylsulfathiazole
C17H13N3O5S2
M + H
404.03694
149.02313
256.02032
9.07
Sulfabenzamide
C13H12N2O3S
M + H
277.06414
156.01138
108.04439
10.32
Sulfacetamide
C8H10N2O3S
M + H
215.04849
173.03792
156.01138
6.73
Sulfachlorpyridazine
C10H9ClN4O2S
M + H
285.02075
156.01138
108.04439
9.25
Sulfachloropyrazine
C10H9ClN4O2S
M + H
285.02075
130.0166
156.01111
10.35
Sulfadiazine
C10H10N4O2S
M + H
251.05972
156.01138
108.04439
7.13
Sulfadimethoxine
C12H14N4O4S
M + H
311.08085
156.07675
108.04439
10.43
Fluoroquinolones
Lomefloxacin
C17H19F2N3O3
M + H
352.14672
308.1569
265.1147
7.58
Marbofloxacin
C17H19FN4O4
M + H
363.14631
320.10411
72.08078
7.17
Nadifloxacin
C19H21FN2O4
M + H
361.15581
343.14389
283.08725
10.76
Nalidixic acid
C12H12N2O3
M + H
233.09207
205.06077
187.0502
11.43
Norfloxacin
C16H18FN3O3
M + H
320.1405
276.15067
233.10847
7.24
Ofloxacin
C18H20FN3O4
M + H
362.15106
318.16123
261.10338
7.31
Orbifloxacin
C19H20F3N3O3
M + H
396.15295
352.16312
295.10527
7.89
Oxolinic acid
C13H11NO5
M + H
262.071
244.06043
234.0397
9.95
Pipemidic acid
C14H17N5O3
M + H
304.14042
290.16632
233.10847
6.75
Pefloxacin
C17H20FN3O3
M + H
334.15615
217.10839
189.0779
7.35
Cinoxacin
C12H10N2O5
M + H
263.06625
235.07133
217.06077
9.47
Sarafloxacin
C20H17F2N3O3
M + H
386.13107
342.14125
299.09905
8.16
Sparfloxacin
C19H22F2N4O3
M + H
393.17327
349.18344
292.12559
8.22
Ciprofloxacin
C17H18FN3O3
M + H
332.1405
288.15067
245.10847
7.37
Danofloxacin
C19H20FN3O3
M + H
358.15615
314.16632
283.12412
7.54
Difloxacin
C21H19F2N3O3
M + H
400.14672
356.15689
299.09905
8.27
Enoxacin
C15H17FN4O3
M + H
321.13575
277.14592
257.13969
7.13
Enrofloxacin
C19H22FN3O3
M + H
360.1718
316.18197
245.10847
7.73
Fleroxacin
C17H18F3N3O3
M + H
370.1373
326.14747
269.08962
7.36
Flumequine
C14H12FNO3
M + H
262.0874
244.07683
220.04045
11.59
Gatifloxacin
C19H22FN3O4
M + H
376.16671
332.17688
289.13468
7.97
Stimulants
Cyproheptadine
C21H21N
M + H
288.17468
191.08553
96.08078
10.67
Fenoterol
C17H21NO4
M + H
304.15433
286.14377
135.08044
6.57
Labetalol
C19H24N2O3
M + H
329.18597
311.1754
294.14886
8.97
Penbutolol
C18H29NO2
M + H
292.22711
236.16451
201.12739
11.08
Phenylethanolamine A
C19H24N2O4
M + H
345.18088
327.17032
150.09134
10.03
Ractopamine
C18H23NO3
M + H
302.17507
284.16451
164.10699
7.56
Salbutamol
C13H21NO3
M + H
240.15942
148.07569
166.08625
5.75
Salmeterol
C25H37NO4
M + H
416.27954
398.26897
380.2584
11.03
Terbutaline
C12H19NO3
M + H
226.14377
170.08117
152.07061
5.71
Mabuterol
C13H18ClF3N2O
M + H
311.11325
237.03951
217.03343
9
Tulobuterol
C12H18ClNO
M + H
228.11497
172.05237
154.0418
8.25
Bambuterol
C18H29N3O5
M + H
368.218
312.1554
294.14483
8.65
Brombuterol
C12H18Br2N2O
M + H
364.98586
290.9127
211.99436
8.71
Cimaterol
C12H17N3O
M + H
220.14444
202.13387
160.08692
5.93
Cimbuterol
C13H19N3O
M + H
234.16009
160.08656
143.06007
6.61
Clenbuterol
C12H18Cl2N2O
M + H
277.0869
259.07633
203.01373
8.31
Clenproperol
C11H16Cl2N2O
M + H
263.07125
245.06068
203.01373
7.85
Clonidine
C9H9Cl2N3
M + H
230.02463
212.99808
/
6.77
Hormones
Chlormadinone acetate
C23H29ClO4
M + H
405.18271
309.1849
267.1743
15.67
17a-methyltestosterone
C20H30O2
M + H
303.23186
285.22129
267.21073
13.63
Clobetasol propionate
C25H32ClFO5
M + H
467.19951
263.143
147.0804
15.08
Clobetasone butyrate
C26H32ClFO5
M + H
479.19951
279.138
343.1459
16.13
Corticosterone
C21H30O4
M + H
347.22169
329.21112
311.20056
11.61
Hydrocortisone
C21H30O5
M + H
363.2166
327.19547
309.18491
10.34
Cortisone acetate
C23H30O6
M + H
403.21152
343.19038
163.11174
12.53
Cortisone
C21H28O5
M + H
361.20095
163.1117
121.0648
10.45
Deflazacort
C25H31NO6
M + H
442.22241
142.0499
312.1958
12.39
Dexamethasone
C22H29FO5
M + H
393.20718
355.19039
337.17982
11.21
Diflorasone diacetate
C26H32F2O7
M + H
495.21889
121.0648
317.1536
13.91
Epitestosterone
C19H28O2
M + H
289.21621
97.0648
109.0648
13.93
Estradiol benzoate
C25H28O3
M + H
377.21112
279.1743
321.1849
12.22
Fludrocortisone acetate
C23H31FO6
M + H
423.21774
181.1023
239.143
12.22
Flumetasone pivalate
C27H36F2O6
M + H
495.25527
57.0699
121.0648
15.25
Flumethasone
C22H28F2O5
M + H
411.19776
235.1117
277.1587
11.2
Fluocinolone acetonide
C24H30F2O6
M + H
453.20832
121.0648
337.1434
11.86
Fluorometholone
C22H29FO4
M + H
377.21226
279.1743
135.0804
12.22
Flurandrenolide
C24H33FO6
M + H
437.23339
361.1798
105.0699
12.01
Fluticasone propionate
C25H31F3O5S
M + H
501.19171
121.0648
275.143
15.08
Nandrolone propionate
C21H30O3
M + H
331.22677
257.18999
239.17943
17.38
Halcinonide
C24H32ClFO5
M + H
455.19951
121.0648
377.1514
14.98
Dihydrodiethylstilbestrol
C18H22O2
M + H
271.16926
109.1117
253.1587
11.92
Medroxyprogesterone
C24H34O4
M + H
387.25299
123.0804
327.2319
15.81
acetate
Megestrol acetate
C24H32O4
M + H
385.23734
267.1743
224.156
15.53
Melengestrol acetate
C25H32O4
M + H
397.23734
279.1743
337.2162
15.82
Methandienone
C20H28O2
M + H
301.21621
283.20564
149.13248
12.73
Methylprednisolone
C22H30O5
M + H
375.2166
161.0961
135.0804
10.99
Norethindrone
C20H26O2
M + H
299.20056
109.0648
281.19
13.12
Nandrolone propionate
C18H26O2
M + H
275.20056
109.06499
239.17885
12.47
Levonorgestrel
C21H28O2
M + H
313.21621
109.0648
245.19
14.23
Prednicarbate
C27H36O8
M + H
489.24829
147.0804
289.1587
14.91
Prednisolone
C21H28O5
M + H
361.20095
147.0804
171.0804
10.2
Prednisone
C21H26O5
M + H
359.1853
341.17474
237.12739
10.27
Progesterone
C21H30O2
M + H
315.23186
109.06479
97.06479
15.76
Dehydrotestosterone
C19H26O2
M + H
287.20056
121.0647
135.1167
12.22
Testosterone
C19H28O2
M + H
289.21621
109.06479
97.06479
13.03
Trenbolone
C18H22O2
M + H
271.16926
253.15869
199.11174
11.92
Triamcinolone
C24H31FO6
M + H
435.21774
397.201
339.1591
11.69
acetonide
Beclomethasone
C22H29ClO5
M + H
409.17763
391.1671
279.1743
11.45
Betamethasone
C28H37FO7
M + H
505.25961
279.1741
319.1693
15.45
dipropionate
Betamethasone
C27H37FO6
M + H
477.26469
279.1743
147.0804
14.55
valerate
Betamethasone
C22H29FO5
M + H
393.20718
355.19039
279.17434
11.14
Nitroimidazoles
Dimetridazole
C5H7N3O2
M + H
142.0611
112.06311
95.06037
7.17
Ipronidazole
C7H11N3O2
M + H
170.0924
140.09441
123.09167
10.33
Metronidazole
C6H9N3O3
M + H
172.07167
128.04545
82.05255
6.39
Ornidazole
C7H10ClN3O3
M + H
220.04835
128.04547
203.14304
8.77
Hydroxydimetridazole
C5H7N3O3
M + H
158.05602
140.0455
110.0475
6.42
Ronidazole
C6H8N4O4
M + H
201.06183
140.04545
110.04746
7.03
Secnidazole
C7H11N3O3
M + H
186.08732
128.0455
111.0427
7.56
Tinidazole
C8H13N3O4S
M + H
248.06995
154.0611
110.08384
8.12
Antiviral
Amantadine
C10H17N
M + H
152.14338
135.11683
107.08553
7.48
drugs
Rimantadine;
C12H21N
M + H
180.17468
163.14778
81.0704
9
Lincosamides
Clindamycin
C18H33ClN2O5S
M + H
425.18715
126.12773
/
8.69
Lincomycin
C18H34N2O6S
M + H
407.221
126.12773
359.21766
6.76
Amphenicols
Chloramphenicol
C11H12C12N2O5
M − H
321.00505
257.03346
194.04588
10.11
Florfenicol
C12H14Cl2FNO4S
M − H
355.99319
335.98696
185.02779
9.96
Thiamphenicol
C12H15Cl2NO5S
M − H
353.99752
290.02593
185.02779
8.27
β-Lactams
Ceftiofur
C19H17N5O7S3
M + H
524.03629
241.03899
210.02065
9.63
Flucloxacillin
C19H17ClFN3O5S
M + H
454.06342
160.04242
114.03742
12.5
Cloxacillin
C19H18ClN3O5S
M + H
436.07285
277.0374
206.0367
12.26
Nafcillin
C21H22N2O5S
M + H
415.13222
199.0754
171.0441
12.54
Piperacillin
C23H27N5O7S
M + H
518.1704
143.0815
115.0502
10.16
Penicillin G
C16H18N2O4S
M + H
335.106
217.06414
176.07061
10.77
Quinoxalines
Quinocetone
C18H14N2O3
M + H
307.10772
143.06018
273.10178
11.99
Antipyretics
Phenacetin
C10H13NO2
M + H
180.10191
110.0602
138.09109
10.11
and analgesics
Salicylic acid
C7H6O3
M − H
137.02442
93.0346
65.0397
3.74
Amidopyrine
C13H17N3O
M + H
232.14444
113.10738
98.08418
6.46
Antipyrine
C11H12N2O
M + H
189.10224
147.09135
161.10696
8.39
Dapsone
C12H12N2O2S
M + H
249.06922
156.01122
108.04431
9.03
Flunixin meglumine
C14H11F3N2O2
M + H
297.08454
279.07397
264.0505
13.66
Acetaminophen
C8H9NO2
M + H
152.07061
110.06004
/
6.25
Psychoactive
Haloperidol
C21H23ClFNO2
M + H
376.14741
358.13685
165.07102
10.3
drugs
Imipramine
C19H24N2
M + H
281.20123
86.0963
236.1434
10.71
Nitrazepam
C15H11N3O3
M + H
282.08732
268.08383
207.09126
11.53
Oxazepam
C15H11ClN2O2
M + H
287.05818
241.05203
269.04703
11.49
Pemoline
C9H8N2O2
M + H
177.06585
106.0651
79.0542
7.74
Perphenazine
C21H26ClN3OS
M + H
404.15579
143.11763
171.14877
10.83
Promethazine
C17H20N2S
M + H
285.142
198.0372
86.09643
10.34
Propionylpromazine
C20H24N2OS
M + H
341.16821
86.0964
58.0651
10.95
hydrochloride
Sulpiride
C15H23N3O4S
M + H
342.1482
214.0169
112.1121
6.21
Xylazine
C12H16N2S
M + H
221.1107
90.0372
164.0528
8.27
hydrochloride
Acepromazin
C19H22N2OS
M + H
327.15256
254.06341
86.09643
10.2
Anisopirol
C19H24FN3O
M + H
330.19762
312.1865
121.076
7.44
Azaperone
C19H22FN3O
M + H
328.18197
165.07069
121.07603
8.04
Carbamazepine
C15H12N2O
M + H
237.10224
194.0964
220.0757
11.15
Chloropromazine
C17H19ClN2S
M + H
319.10302
86.09643
246.01379
11.25
Diazepam
C16H13ClN2O
M + H
285.07892
154.0415
193.0883
13.58
Diphenhydramine
C17H21NO
M + H
256.16959
167.0855
152.0621
10.03
hydrochloride
Droperidol
C22H22FN3O2
M + H
380.17688
165.07072
194.09726
9.35
Estazolam
C16H11ClN4
M + H
295.0745
267.05524
205.0755
11.44
Macrolides
Clarithromycin
C38H69NO13
M + H
748.48417
158.11756
116.07061
11.04
Tiamulin
C28H47NO4S
M + H
494.32986
192.10528
119.01613
10.8
Erythromycin
C37H67NO13
M + H
734.46852
158.11756
116.07061
9.92
Kitasamycin
C40H67NO14
M + H
786.46343
558.32727
174.11247
11.25
Tilmicosin
C46H80N2O13
M + H
869.57332
174.11247
88.07569
8.93
Tylosin
C46H77NO17
M + H
916.52643
772.44778
174.11247
10.17
anthelmintics
Mebendazole
C16H13N3O3
M + H
296.10297
264.07675
105.03349
10.85
Mebendazole-amine
C14H11N3O
M + H
238.09749
105.03369
/
8.45
2-aminofluorobenzimidazole
C14H10FN3O
M + H
256.08807
123.0241
113.0397
8.74
Oxfendazole
C15H13N3O3S
M + H
316.07504
284.04882
223.0576
9.26
Oxibendazole
C12H15N3O3
M + H
250.11862
218.0924
176.04545
9.33
Parbendazole
C13H17N3O2
M + H
248.13935
216.1131
160.0505
10.65
5-hydroxythiabendazole
C10H7N3OS
M + H
218.03826
191.02736
/
6.44
Tiabendazole
C10H7N3S
M + H
202.04334
175.03245
131.06037
7.12
Albendazole
C12H15N3O2S
M + H
266.09577
234.06956
191.01478
10.99
Albendazole sulfone
C12H15N3O4S
M + H
298.0856
266.05939
224.01244
9.4
Albendazole sulfoxide
C12H15N3O3S
M + H
282.09069
240.04347
208.01752
8.08
Amino albendazole
C10H13N3O2S
M + H
240.08012
198.03317
165.05328
6.94
sulfone
Benzimidazole
C7H6N2
M + H
119.06037
92.0495
65.0386
4.8
Febantel
C20H22N4O6S
M + H
447.13328
383.08085
280.05391
14.78
Lobendazole
C10H11N3O2
M + H
206.0924
160.0505
178.0609
7.59
toltrazuril sulfoxide
C18H14F3N3O5S
M − H
440.05335
371.05813
/
8.97
Clopidol
C7H7Cl2NO
M + H
191.99775
86.9996
101.01525
6.83
Dinitolmide
C8H7N3O5
M − H
224.03129
181.02438
77.03858
9.91
Halofuginone
C16H17BrClN3O3
M + H
414.02146
100.07598
120.08076
8.89
Levamisole
C11H12N2S
M + H
205.0794
178.0685
/
6.99
Pesticides
Buprofezin
C16H23N3OS
M + H
306.16346
201.10561
116.05285
17.73
Carboxin
C12H13NO2S
M + H
236.07398
143.01613
93.0573
12.61
3-hydroxycarbofuran
C12H15NO4
M + H
238.10738
163.07536
135.08044
9.09
Clothianidin
C6H8ClN5O2S
M + H
250.016
131.96692
113.0168
8.96
Cyromazine
C6H10N6
M + H
167.10397
85.05087
125.08217
3.63
Diuron
C9H10Cl2N2O
M + H
233.02429
72.04439
159.97153
12.65
Ethopabate
C12H15NO4
M + H
238.10738
206.08117
164.07061
10.29
Fipronil
C12H4Cl2F6N4OS
M − H
434.93143
329.95845
249.95853
15.66
Fluridone
C19H14F3NO
M + H
330.11003
310.1038
290.09757
13.62
Acephate
C4H10NO3PS
M + H
184.01918
142.99264
112.99968
5.61
Hexazinone
C12H20N4O2
M + H
253.1659
171.08765
71.06037
10.59
Imazalil
C14H14C12N2O
M + H
297.0556
158.97628
255.00864
10.77
Imidacloprid
C9H10ClN5O2
M + H
256.05958
209.05885
175.09793
9.3
Linuron
C9H10Cl2N2O2
M + H
249.01921
159.97153
182.02414
14.09
Metribuzin
CSH14N4OS
M + H
215.09611
187.10119
131.03859
11.73
Myclobutanil
C15H17ClN4
M + H
289.12145
70.03997
125.01525
14.21
Acetamiprid
C10H11ClN4
M + H
223.0745
126.0105
98.9997
9.58
Norflurazon
C12H9ClF3N3O
M + H
304.0459
284.03967
160.03686
12.81
Propyzamide
C12H11Cl2NO
M + H
256.02905
189.9821
172.95555
14.68
Atrazine
C8H14ClN5
M + H
216.10105
174.0541
96.05562
12.63
Simazine
C7H12ClN5
M + H
202.0854
132.0323
104.001
11.35
Desethyl atrazine
C6H10ClN5
M + H
188.06975
146.0228
104.001
9.37
Azoxystrobin
C22H17N3O5
M + H
404.1241
344.10397
329.07949
14.2
Benoxacor
C11H11Cl2NO2
M + H
260.02396
149.08352
120.04439
14.31
Other
Scopolamine
C17H21NO4
M + H
304.15433
156.10191
138.09134
7
substances
Valnemulin
C31H52N2O5S
M + H
565.36697
263.1417
72.08078
11.15
Atropine
C17H23NO3
M + H
290.17507
124.11208
93.06988
7.61
(6) analyzing the filtrate by the ultra high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometer to obtain original data of the sample;
(7) subjecting the original data of the sample to automatic extraction using Trace Finder software within a mass window of 5 ppm;
wherein when a compound meets the following conditions at the same time, it indicates that the compound is a suspected positive compound in the sample:
(i) a signal-noise ratio (S/N) of the compound is greater than 3;
(ii) a difference between the measured retention time of the compound and the retention time of the compound in the mass spectrometry database is equal to or less than 0.2 min or within ±2.5% (not to exceed 0.5 min);
(iii) the measured parent ion and one fragment ion of the compound simultaneously match the information in the mass spectrometry database, and a mass accuracy of the parent ion is less than 5 ppm and a mass accuracy of the fragment ion is less than 10 ppm;
and
(8) comparing a fragment ion mass spectrometry of the suspected positive compound in the sample with a fragmentation mass spectrometry of standard for further identification;
wherein if the mass accuracy between main fragment ions in the two fragment ion mass spectrometries is less than 10 ppm and the main fragment ions in the two fragment ion mass spectrometries have identical relative abundance, it confirms that the suspected positive compound is present in the sample.

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Screening and confirmation method for veterinary drugs and additives in animal-derived food

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Screening and confirmation method for veterinary drugs and additives in animal-derived food

Life of this patent

Abstract

Claims6