California Cannabis Pesticides and Mycotoxins in Gummy Edibles on Raptor ARC-18
California Cannabis Pesticides and Mycotoxins in Gummy Edibles on Raptor ARC-18
Peaks
tR (min)
Precursor Ion
Product Ion 1
Product Ion 2
Polarity
1.
Daminozide-d6
0.7
167.0
149.3
49.3
+
2.
Daminozide
0.7
161.1
44.1
143.2
+
3.
Acephate
1.7
184.0
143.1
95.1
+
4.
Oxamyl
2.0
237.1
72.1
90.1
+
5.
Flonicamid
2.1
230.1
203.1
174.1
+
6.
Methomyl
2.1
163.1
88.1
106.1
+
7.
Thiamethoxam
2.1
292.0
211.1
181.1
+
8.
Imidacloprid
2.3
256.1
209.1
175.1
+
9.
Mevinphos
2.4
225.1
127.1
193.2
+
10.
Acetamiprid
2.4
223.0
126.1
56.1
+
11.
Dimethoathe-d6
2.4
236.1
205.1
-
+
12.
Dimethoate
2.4
230.0
199.1
125.1
+
13.
Thiacloprid
2.5
253.0
126.0
90.1
+
14.
Aflatoxin G2
2.5
331.2
189.3
115.2
+
15.
Aflatoxin G1
2.5
329.2
243.2
215.3
+
16.
Aldicarb
2.6
116.0
89.2
70.2
+
17.
Aflatoxin B2
2.6
315.3
287.2
243.3
+
18.
Dichlorvos
2.7
220.9
109.1
79.2
+
19.
Dichlorvos-d6
2.7
227.0
115.1
-
+
20.
Aflatoxin B1
2.7
313.2
241.2
128.2
+
21.
Imazalil
2.7
297.0
159.0
201.0
+
22.
Carbofuran
2.7
222.1
123.1
165.2
+
23.
Propoxur
2.7
210.1
111.1
93.1
+
24.
Carbaryl-d7
2.8
209.2
152.2
-
+
25.
Carbaryl
2.8
202.1
145.1
127.1
+
26.
Diuron-d6
3.0
239.1
78.2
-
+
27.
Atrazine-d5
3.0
221.2
179.1
-
+
28.
Naled
3.1
397.8
127.1
109.1
+
29.
Metalaxyl
3.1
280.2
220.2
192.2
+
30.
Spiroxamine
3.1
298.3
144.2
100.2
+
31.
Chlorantraniliprole
3.2
483.9
452.9
285.9
+
32.
Phosmet
3.2
318.0
160.1
77.2
+
33.
Azoxystrobin
3.3
404.0
372.1
344.1
+
34.
Linuron-d6
3.3
255.1
160.1
-
+
35.
Fludioxonil
3.4
247.0
180.0
126.0
-
36.
Methiocarb
3.4
226.1
169.1
121.1
+
37.
Dimethomorph
3.5
388.2
301.2
165.3
+
38.
Boscalid
3.5
342.9
307.1
140.1
+
39.
Paclobutrazol
3.6
294.3
70.1
125.1
+
40.
Malathion
3.6
331.0
127.2
285.2
+
41.
Myclobutanil
3.7
289.1
70.1
125.1
+
42.
Bifenazate
3.7
301.0
198.1
170.2
+
43.
Ochratoxin A
3.8
404.2
239.1
358.3
+
44.
Fenhexamid
3.9
302.1
97.1
55.2
+
45.
Spirotetramat
4.0
374.2
302.1
216.1
+
46.
Ethoprophos
4.1
243.1
131.1
97.1
+
47.
Fipronil
4.1
436.8
331.8
251.9
-
48.
Fenoxycarb
4.2
302.1
88.1
116.1
+
49.
Kresoxim-methyl
4.4
314.2
267.2
222.2
+
50.
Tebuconazole
4.4
308.1
70.1
125.1
+
51.
Diazinon-d10
4.6
315.2
170.2
-
+
52.
Spinosyn A (Spinosad)
4.6
732.4
142.2
98.1
+
53.
Diazinon
4.6
305.1
169.2
153.2
+
54.
Coumaphos
4.7
363.1
227.1
307.1
+
55.
Pyridaben
4.7
365.1
309.2
147.2
+
56.
Propiconazole
4.7
342.0
159.0
69.2
+
57.
Clofentezine
4.8
303.0
138.1
102.1
+
58.
Spinosyn D (Spinosad)
5.0
746.5
142.3
98.4
+
59.
Spinosyn J (Spinetoram)
5.1
748.5
142.3
98.3
+
60.
Trifloxystrobin
5.3
409.2
186.1
145.1
+
61.
Prallethrin
5.3
301.2
123.2
105.2
+
62.
Pyrethrin II
5.5
373.1
161.1
133.2
+
63.
Spinosyn L (Spinetoram)
5.6
760.5
142.2
98.1
+
64.
Piperonyl butoxide
6.0
356.3
177.2
119.2
+
65.
Chlorpyrifos
6.1
349.9
198.0
97.1
+
66.
Hexythiazox
6.2
353.1
228.1
168.1
+
67.
Etoxazole
6.6
360.2
141.1
304.2
+
68.
Spiromesifen
6.7
273.2
255.2
187.2
+
69.
Pyrethrin I
6.9
329.2
161.2
105.2
+
70.
Cyfluthrin (qualifier)
6.9
453.1
193.2
-
+
71.
Cyfluthrin
6.9
451.1
191.2
-
+
72.
Cypermethrin
7.1
433.1
191.0
416.0
+
73.
Fenpyroximate
7.1
422.2
366.1
138.1
+
74.
trans-Permethrin
7.6
408.3
183.2
355.1
+
75.
cis-Permethrin
7.9
408.3
183.2
355.1
+
76.
Avermectin B1a
7.9
890.5
305.4
567.4
+
77.
Etofenprox
8.0
394.3
177.2
359.3
+
78.
Bifenthrin
8.2
440.0
181.2
166.2
+
79.
Acequinocyl (precursor ion 1)
9.4
402.3
343.2
189.0
+
80.
Acequinocyl (precursor ion 2)
9.4
386.0
344.2
189.1
+
LC_GN0666
Column
Raptor ARC-18 (cat.# 9314A12)
Dimensions:
100 mm x 2.1 mm ID
Particle Size:
2.7 µm
Pore Size:
90 Å
Guard Column:
Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 µm (cat.# 9314A0252)
Temp.:
40 °C
Sample
California pesticide standard #1 (cat.# 34124)
California pesticide standard #2 (cat.# 34125)
California pesticide standard #3 (cat.# 34126)
California pesticide standard #4 (cat.# 34127)
California pesticide standard #5 (cat.# 34128)
California pesticide standard #6 (cat.# 34129)
Dimethoate-d6 (cat.# 31988)
Dichlorvos-d6 (cat.# 31987)
Carbaryl-d7 (cat.# 31985)
Diazinon-d10 (cat.# 31986)
Atrazine-d5 (cat.# 31984)
Diuron-d6 (cat.# 31989)
Liuron-d6 (cat.# 31990)
Aflatoxins standard (cat.# 34121)
Ochratoxin A (cat.# 34122)
Compounds not present in these mixes were obtained separately.
Diluent:
75:25 Acetonitrile:water
Conc.:
3.75-15 ng/mL (Expected concentration range in extract of gummy initially spiked at 100 ng/g.)
Inj. Vol.:
2 µL
Mobile Phase
A:
Water, 2 mM ammonium formate, 0.1% formic acid
B:
Methanol, 2 mM ammonium formate, 0.1% formic acid
Time (min)
Flow (mL/min)
%A
%B
0.00
0.5
95
5
1.5
0.5
35
65
8.5
0.5
5
95
9.5
0.5
0
100
10.5
0.5
0
100
10.6
0.5
95
5
12.0
0.5
95
5
Detector
MS/MS
Ion Mode:
ESI+/ESI-
Mode:
MRM
Instrument
UHPLC
Notes
Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by a 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 750 µL of organic extract was mixed with 250 µL of water. 2 μL of final extract was injected into the LC-MS/MS system.
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