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California Cannabis Pesticides and Mycotoxins in Dried Hemp on Raptor ARC-18

LC_GN0682
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2Polarity
1.Daminozide1.2161.1143.244.1+
2.Daminozide-d61.2167.0149.3+
3.Acephate2.5184.0143.195.1+
4.Oxamyl2.8237.172.190.1+
5.Flonicamid2.9230.1203.1174.1+
6.Methomyl2.9163.188.1106.1+
7.Thiamethoxam2.9292.0211.1181.1+
8.Imidacloprid3.2256.1209.1175.1+
9.Clothianidin3.2250.1169.2132.3+
10.Dimethoate-d63.3236.1205.1+
11.Mevinphos I3.3225.1127.1193.2+
12.Dimethoate3.4230.0199.1125.1+
13.Acetamiprid3.4223.0126.156.1+
14.Thiacloprid3.7253.0126.090.1+
15.Mevinphos II3.7225.1127.1193.2+
16.Aflatoxin G23.7331.2189.3115.2+
17.Aflatoxin G14.0329.2243.2215.3+
18.Aldicarb4.0208.4116.089.0+
19.Aflatoxin B24.4315.3287.2243.3+
20.Dichlorvos (DDVP)4.6220.9108.879.2+
21.Propoxur (Baygon)4.7210.1111.193.1+
22.Aflatoxin B14.8313.2241.2128.2+
23.Carbofuran4.8222.1123.1165.2+
24.Carbary-d75.0209.2125.2+
25.Carbaryl (Sevin)5.1202.1145.1127.1+
26.Imazalil5.2297.0159.0201.0+
27.Atrazine-d55.7221.2179.1+
28.Diuron-d65.8239.178.2+
29.Metalaxyl5.9280.2220.2192.2+
30.Naled6.0397.8127.1109.1+
31.Chlorantraniliprole6.1483.9452.9285.9+
32.Phosmet6.2318.0160.177.2+
33.Spiroxamine6.3298.3144.2100.2+
34.Linuron-d66.3255.1160.1+
35.Azoxystrobin6.6404.0372.1344.1+
36.Methiocarb6.6226.1169.1121.1+
37.Fludioxonil6.6274.0180.0126.0-
38.Dimethomorph I6.8388.2301.2165.3+
39.Boscalid6.8342.9307.5140.1+
40.Paclobutrazol7.0294.370.1125.1+
41.Malathion7.0331.0127.2285.2+
42.Dimethomorph II7.2388.2301.2165.3+
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2Polarity
43.Myclobutanil7.3289.170.1125.1+
44.Bifenazate7.5301.0198.1170.2+
45.Ochratoxin A7.6404.2239.1358.3+
46.Fenhexamid7.8302.197.155.2+
47.Spirotetramat8.2374.2216.1302.1+
48.Ethoprophos8.3243.1131.197.1+
49.Fipronil8.7436.8331.8251.9-
50.Fenoxycarb8.9302.188.1116.1+
51.Kresoxim methyl9.3314.2267.2222.2+
52.Tebuconazole9.5308.170.1125.1+
53.Diazinon-d109.7315.2170.2+
54.Diazinon9.8305.1169.2153.2+
55.Coumaphos10.1363.1227.1307.1+
56.Propiconazole (Tilt)10.1342.0159.069.2+
57.Clofentezine10.2303.0138.1102.1+
58.Spinosad (Spinosyn A)10.8732.4142.298.1+
59.MGK-264 I11.1276.2210.1121.1+
60.Prallethrin11.6301.2123.2104.9+
61.Trifloxystrobin11.6409.2186.1145.1+
62.Spinosad (Spinosyn D)11.8746.5142.398.4+
63.Spinetoram (Spinosyn J)12.1748.5142.598.3+
64.Pyrethrins (Pyrethrin II)12.1373.1161.1133.2+
65.Spinetoram (Spinosyn L)13.2760.5142.298.1+
66.Piperonyl butoxide-d913.2365.4177.4+
67.Piperonyl butoxide13.3356.3177.2119.2+
68.Chlorpyrifos13.4349.9198.097.1+
69.Hexythiazox13.7353.1228.1168.1+
70.Etoxazole14.6360.2141.1304.2+
71.Spiromesifen14.7388.4273.3255.3+
72.Pyrethrins (Pyrethrin I)15.1329.2161.2133.2+
73.Cyfluthrin15.3451.1191.2+
74.Cyfluthrin (qualifier)15.3453.1193.2+
75.Cypermethrin15.6433.1191.0416.0+
76.Fenpyroximate15.7422.2366.1138.1+
77.Pyridaben16.3365.1147.2309.2+
78.Permethrin (trans)16.6408.3183.2355.1+
79.Permethrin (cis)16.9408.3183.2355.1+
80.Abamectin16.9890.5305.4567.4+
81.Etofenprox17.0394.3177.2359.3+
82.Bifenthrin-d617.1446.3181.3+
83.Bifenthrin17.2440.0181.2166.2+
84.Acequinocyl18.2402.3343.2189.0+
ColumnRaptor ARC-18 (cat.# 9314A62)
Dimensions:150 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, 5 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)
Aflatoxins (B1, B2, G1, G2) Standard (cat.# 34121)
Ochratoxin A (cat.# 34122)
Dimethoate-d6 (cat.# 31988)
Carbaryl-d7 (cat.# 31985)
Diazinon-d10 (diethyl-d10) (cat.# 31986)
Atrazine-d5 (cat.# 31984)
Diuron-d6 (cat.# 31989)
Linuron-d6 (cat.# 31990)
Compounds not present in these mixes were obtained separately.
Diluent:67.4:21.2:11.4 Acetonitrile:methanol:water
Conc.:6-12 ng/mL (Expected concentration range in extract of hemp initially spiked at 100 ng/g.)
Inj. Vol.:1.5 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
0.000.4955
1.00.45050
2.50.45050
4.00.43565
7.00.43565
7.50.43070
9.00.43070
9.50.42575
11.00.42575
11.50.42080
13.50.42080
15.50.4595
16.50.40100
19.50.40100
19.60.4955
DetectorMS/MS
Ion Source:Electrospray
Ion Mode:ESI+/ESI-
Mode:MRM
InstrumentShimadzu Nexera X2
Sample Preparation1 g of pulverized hemp was weighed in a 15 mL polypropylene tube and fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 100 ng/g. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample followed by a 5 min vortex extraction at 2500 rpm. 200 µL of water was added to a 6 mL hydrophilic lipophilic balanced (HLB) cartridge (200 mg) (Restek cat.# 28451). Then, 3 mL of hemp extract was transferred to the cartridge. Vacuum was applied to collect the cleaned extract. After collecting all the sample, the vacuum was stopped, and 300 µL of methanol was added to help elute all the target analytes (vacuum was reapplied and the rinsing solvent was collected with the rest of the extract). 600 µL of extract was mixed with 400 µL of 2:2:1 methanol:acetonitrile(1% acetic acid):water. 1.5 μL of final extract was injected into the LC-MS/MS system.
NotesAutosampler temperature: 10 °C