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

LC_GN0675
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2Polarity
1.Daminozide-d60.7167.0149.349.3+
2.Daminozide0.7161.144.1143.2+
3.Acephate1.7184.0143.195.1+
4.Oxamyl2.0237.172.190.1+
5.Flonicamid2.1230.1203.1174.1+
6.Methomyl2.1163.188.1106.1+
7.Thiamethoxam2.1292.0211.1181.1+
8.Imidacloprid2.3256.1209.1175.1+
9.Mevinphos2.4225.1127.1193.2+
10.Acetamiprid2.4223.0126.156.1+
11.Dimethoathe-d62.4236.1205.1-+
12.Dimethoate2.4230.0199.1125.1+
13.Thiacloprid2.5253.0126.090.1+
14.Aflatoxin G22.5331.2189.3115.2+
15.Aflatoxin G12.5329.2243.2215.3+
16.Aldicarb2.6116.089.270.2+
17.Aflatoxin B22.6315.3287.2243.3+
18.Dichlorvos2.7220.9109.179.2+
19.Dichlorvos-d62.7227.0115.1-+
20.Aflatoxin B12.7313.2241.2128.2+
21.Imazalil2.7297.0159.0201.0+
22.Carbofuran2.7222.1123.1165.2+
23.Propoxur2.7210.1111.193.1+
24.Carbaryl-d72.8209.2152.2-+
25.Carbaryl2.8202.1145.1127.1+
26.Diuron-d63.0239.178.2-+
27.Atrazine-d53.0221.2179.1-+
28.Naled3.1397.8127.1109.1+
29.Metalaxyl3.1280.2220.2192.2+
30.Spiroxamine3.1298.3144.2100.2+
31.Chlorantraniliprole3.2483.9452.9285.9+
32.Phosmet3.2318.0160.177.2+
33.Azoxystrobin3.3404.0372.1344.1+
34.Linuron-d63.3255.1160.1-+
35.Fludioxonil3.4247.0180.0126.0-
36.Methiocarb3.4226.1169.1121.1+
37.Dimethomorph3.5388.2301.2165.3+
38.Boscalid3.5342.9307.1140.1+
39.Paclobutrazol3.6294.370.1125.1+
40.Malathion3.6331.0127.2285.2+
41.Myclobutanil3.7289.170.1125.1+
42.Bifenazate3.7301.0198.1170.2+
43.Ochratoxin A3.8404.2239.1358.3+
44.Fenhexamid3.9302.197.155.2+
45.Spirotetramat4.0374.2302.1216.1+
46.Ethoprophos4.1243.1131.197.1+
47.Fipronil4.1436.8331.8251.9-
48.Fenoxycarb4.2302.188.1116.1+
49.Kresoxim-methyl4.4314.2267.2222.2+
50.Tebuconazole4.4308.170.1125.1+
51.Diazinon-d10 4.6315.2170.2-+
52.Spinosyn A (Spinosad)4.6732.4142.298.1+
53.Diazinon4.6305.1169.2153.2+
54.Coumaphos4.7363.1227.1307.1+
55.Pyridaben4.7365.1309.2147.2+
56.Propiconazole4.7342.0159.069.2+
57.Clofentezine4.8303.0138.1102.1+
58.Spinosyn D (Spinosad)5.0746.5142.398.4+
59.Spinosyn J (Spinetoram)5.1748.5142.398.3+
60.Trifloxystrobin5.3409.2186.1145.1+
61.Prallethrin5.3301.2123.2105.2+
62.Pyrethrin II5.5373.1161.1133.2+
63.Spinosyn L (Spinetoram)5.6760.5142.298.1+
64.Piperonyl butoxide6.0356.3177.2119.2+
65.Chlorpyrifos6.1349.9198.097.1+
66.Hexythiazox6.2353.1228.1168.1+
67.Etoxazole6.6360.2141.1304.2+
68.Spiromesifen6.7273.2255.2187.2+
69.Pyrethrin I6.9329.2161.2105.2+
70.Cyfluthrin (qualifier)6.9453.1193.2-+
71.Cyfluthrin6.9451.1191.2-+
72.Cypermethrin7.1433.1191.0416.0+
73.Fenpyroximate7.1422.2366.1138.1+
74.trans-Permethrin7.6408.3183.2355.1+
75.cis-Permethrin7.9408.3183.2355.1+
76.Avermectin B1a7.9890.5305.4567.4+
77.Etofenprox8.0394.3177.2359.3+
78.Bifenthrin8.2440.0181.2166.2+
79.Acequinocyl (precursor ion 1)9.4402.3343.2189.0+
80.Acequinocyl (precursor ion 2)9.4386.0344.2189.1+
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
Standard/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.:8.8-12.5 ng/mL Expected concentration range (70-100% recovery) in extract of chocolate 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
12.00.5955
DetectorMS/MS
Ion Mode:ESI+/ESI-
Mode:MRM
InstrumentUHPLC
NotesChocolate was pulverized using a SPEX Freezer/Mill grinder, and a 0.5 g sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. Then, 0.5 mL of isopropyl alcohol was added to the sample. The sample was vortexed for 10 sec or until a homogenous mixture was obtained. Afterwards, 2.5 mL of acetonitrile acidified with acetic acid at 1% v/v was added to the vial. Once again, the mixture was vortexed for 30 sec, and then centrifuged for 5 min at 4300 ×g at room temperature. A total of 2 mL of the supernatant was passed through a 100 mg Resprep C18 SPE cartridge (cat.# 26030). 750 µL of organic extract was mixed with 250 µL of water, and the mix was centrifuged for 5 min at 4 °C to precipitate the undissolved fat. 2 μL of final extract was injected into the LC-MS/MS system.