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California Cannabis Pesticides and Mycotoxins in Brownies on Raptor ARC-18

LC_GN0602
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2Polarity
1.Daminozide-d60.6167.0149.349.3+
2.Daminozide0.7161.144.1143.2+
3.Acephate1.5184.0143.195.1+
4.Oxamyl1.8237.172.190.1+
5.Flonicamid1.9230.1203.1174.1+
6.Methomyl1.9163.188.1106.1+
7.Thiamethoxam1.9292.0211.1181.1+
8.Imidacloprid2.2256.1209.1175.1+
9.Mevinphos I2.2225.1127.1193.2+
10.Acetamiprid2.2223.0126.156.1+
11.Dimethoathe-d62.2236.1205.1-+
12.Dimethoate2.3230.0199.1125.1+
13.Thiacloprid2.4253.0126.090.1+
14.Mevinphos II2.4225.1127.1193.2+
15.Aflatoxin G22.4331.2189.3115.2+
16.Aflatoxin G12.4329.2243.2215.3+
17.Aldicarb2.5116.089.270.2+
18.Aflatoxin B22.5315.3287.2243.3+
19.Dichlorvos2.6220.9109.179.2+
20.Dichlorvos-d62.6227.0115.1-+
21.Aflatoxin B12.6313.2241.2128.2+
22.Imazalil2.6297.0159.0201.0+
23.Carbofuran2.6222.1123.1165.2+
24.Propoxur2.6210.1111.193.1+
25.Carbaryl-d72.7209.2152.2-+
26.Carbaryl2.7202.1145.1127.1+
27.Diuron-d62.9239.178.2-+
28.Atrazine-d52.9221.2179.1-+
29.Naled2.9397.8127.1109.1+
30.Metalaxyl2.9280.2220.2192.2+
31.Spiroxamine2.9298.3144.2100.2+
32.Chlorantraniliprole3.0483.9452.9285.9+
33.Phosmet3.0318.0160.177.2+
34.Azoxystrobin3.1404.0372.1344.1+
35.Linuron-d63.1255.1160.1-+
36.Fludioxonil3.2247.0180.0126.0-
37.Methiocarb3.2226.1169.1121.1+
38.Dimethomorph I3.2388.2301.2165.3+
39.Boscalid3.2342.9307.1140.1+
40.Paclobutrazol3.3294.370.1125.1+
41.Malathion3.3331.0127.2285.2+
42.Dimethomorph II3.4388.2301.2165.3+
43.Myclobutanil3.4289.170.1125.1+
44.Bifenazate3.4301.0198.1170.2+
45.Ochratoxin A3.5404.2239.1358.3+
46.Fenhexamid3.5302.197.155.2+
47.Spirotetramat3.7374.2302.1216.1+
48.Ethoprophos3.8243.1131.197.1+
49.Fipronil3.8436.8331.8251.9-
50.Fenoxycarb3.9302.188.1116.1+
51.Kresoxim-methyl4.1314.2267.2222.2+
52.Tebuconazole4.2308.170.1125.1+
53.Diazinon-d10 4.2315.2170.2-+
54.Spinosyn A (spinosad)4.3732.4142.298.1+
55.Diazinon4.3305.1169.2153.2+
56.Coumaphos4.4363.1227.1307.1+
57.Pyridaben4.4365.1309.2147.2+
58.Propiconazole4.4342.0159.069.2+
59.Clofentezine4.5303.0138.1102.1+
60.Spinosyn D (spinosad)4.8746.5142.398.4+
61.Spinosyn J (spinetoram)4.8748.5142.398.3+
62.Trifloxystrobin4.9409.2186.1145.1+
63.Prallethrin4.9301.2123.2105.2+
64.Pyrethrin II5.2373.1161.1133.2+
65.Spinosyn L (spinetoram)5.4760.5142.298.1+
66.Piperonyl butoxide5.7356.3177.2119.2+
67.Chlorpyrifos5.8349.9198.097.1+
68.Hexythiazox5.9353.1228.1168.1+
69.Etoxazole6.4360.2141.1304.2+
70.Spiromesifen6.4273.2255.2187.2+
71.Pyrethrin I6.6329.2161.2105.2+
72.Cyfluthrin (qualifier)6.6453.1193.2-+
73.Cyfluthrin6.6451.1191.2-+
74.Cypermethrin6.8433.1191.0416.0+
75.Fenpyroximate6.8422.2366.1138.1+
76.trans-Permethrin7.4408.3183.2355.1+
77.cis-Permethrin7.7408.3183.2355.1+
78.Avermectin B1a7.7890.5305.4567.4+
79.Etofenprox7.8394.3177.2359.3+
80.Bifenthrin8.0440.0181.2166.2+
81.Acequinocyl (precursor ion 1)9.3402.3343.2189.0+
82.Acequinocyl (precursor ion 2)9.3386.0344.2189.1+
ColumnRaptor 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
SampleCalifornia 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.:5-15 ng/mL (Expected concentration range in extract of brownie 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
0.000.5955
1.50.53565
8.50.5595
9.50.50100
10.50.50100
10.60.5955
120.5955
DetectorMS/MS
Ion Mode:ESI+/ESI-
Mode:MRM
InstrumentUHPLC
NotesBrownies were pulverized using a SPEX Freezer/Mill grinder and 0.5 g samples were fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. 1.5 mL of acetonitrile acidified with 1% acetic acid was added to the sample. The sample was vortexed and sonicated for 5 min, and then the supernatant was passed through a 100 mg Resprep C18 SPE cartridge (cat.# 26030). An additional 1.5 mL of extraction solvent (acidified acetonitrile) was added to the sample pellet, and then the sample was vortexed again. The supernatant was passed through the same C18 cartridge. 750 µL of extract was mixed with 250 µL of water, and then centrifuged for 5 min at low temperature (~7 ⁰C). 2 μL of final extract was injected into the LC-MS/MS system.