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

	Peaks	t_R (min)	Precursor Ion	Product Ion 1	Product Ion 2	Polarity
1.	Daminozide	1.2	161.1	143.2	44.1	+
2.	Daminozide-d6	1.2	167.0	149.3		+
3.	Acephate	2.5	184.0	143.1	95.1	+
4.	Oxamyl	2.8	237.1	72.1	90.1	+
5.	Flonicamid	2.9	230.1	203.1	174.1	+
6.	Methomyl	2.9	163.1	88.1	106.1	+
7.	Thiamethoxam	2.9	292.0	211.1	181.1	+
8.	Imidacloprid	3.2	256.1	209.1	175.1	+
9.	Clothianidin	3.2	250.1	169.2	132.3	+
10.	Dimethoate-d6	3.3	236.1	205.1		+
11.	Mevinphos I	3.3	225.1	127.1	193.2	+
12.	Dimethoate	3.4	230.0	199.1	125.1	+
13.	Acetamiprid	3.4	223.0	126.1	56.1	+
14.	Thiacloprid	3.7	253.0	126.0	90.1	+
15.	Mevinphos II	3.7	225.1	127.1	193.2	+
16.	Aflatoxin G2	3.7	331.2	189.3	115.2	+
17.	Aflatoxin G1	4.0	329.2	243.2	215.3	+
18.	Aldicarb	4.0	208.4	116.0	89.0	+
19.	Aflatoxin B2	4.4	315.3	287.2	243.3	+
20.	Dichlorvos (DDVP)	4.6	220.9	108.8	79.2	+
21.	Propoxur (Baygon)	4.7	210.1	111.1	93.1	+
22.	Aflatoxin B1	4.8	313.2	241.2	128.2	+
23.	Carbofuran	4.8	222.1	123.1	165.2	+
24.	Carbary-d7	5.0	209.2	125.2		+
25.	Carbaryl (Sevin)	5.1	202.1	145.1	127.1	+
26.	Imazalil	5.2	297.0	159.0	201.0	+
27.	Atrazine-d5	5.7	221.2	179.1		+
28.	Diuron-d6	5.8	239.1	78.2		+
29.	Metalaxyl	5.9	280.2	220.2	192.2	+
30.	Naled	6.0	397.8	127.1	109.1	+
31.	Chlorantraniliprole	6.1	483.9	452.9	285.9	+
32.	Phosmet	6.2	318.0	160.1	77.2	+
33.	Spiroxamine	6.3	298.3	144.2	100.2	+
34.	Linuron-d6	6.3	255.1	160.1		+
35.	Azoxystrobin	6.6	404.0	372.1	344.1	+
36.	Methiocarb	6.6	226.1	169.1	121.1	+
37.	Fludioxonil	6.6	274.0	180.0	126.0	-
38.	Dimethomorph I	6.8	388.2	301.2	165.3	+
39.	Boscalid	6.8	342.9	307.5	140.1	+
40.	Paclobutrazol	7.0	294.3	70.1	125.1	+
41.	Malathion	7.0	331.0	127.2	285.2	+
42.	Dimethomorph II	7.2	388.2	301.2	165.3	+
43.	Myclobutanil	7.3	289.1	70.1	125.1	+
44.	Bifenazate	7.5	301.0	198.1	170.2	+
45.	Ochratoxin A	7.6	404.2	239.1	358.3	+
46.	Fenhexamid	7.8	302.1	97.1	55.2	+
47.	Spirotetramat	8.2	374.2	216.1	302.1	+
48.	Ethoprophos	8.3	243.1	131.1	97.1	+
49.	Fipronil	8.7	436.8	331.8	251.9	-
50.	Fenoxycarb	8.9	302.1	88.1	116.1	+
51.	Kresoxim methyl	9.3	314.2	267.2	222.2	+
52.	Tebuconazole	9.5	308.1	70.1	125.1	+
53.	Diazinon-d10	9.7	315.2	170.2		+
54.	Diazinon	9.8	305.1	169.2	153.2	+
55.	Coumaphos	10.1	363.1	227.1	307.1	+
56.	Propiconazole (Tilt)	10.1	342.0	159.0	69.2	+
57.	Clofentezine	10.2	303.0	138.1	102.1	+
58.	Spinosad (Spinosyn A)	10.8	732.4	142.2	98.1	+
59.	MGK-264 I	11.1	276.2	210.1	121.1	+
60.	Prallethrin	11.6	301.2	123.2	104.9	+
61.	Trifloxystrobin	11.6	409.2	186.1	145.1	+
62.	Spinosad (Spinosyn D)	11.8	746.5	142.3	98.4	+
63.	Spinetoram (Spinosyn J)	12.1	748.5	142.5	98.3	+
64.	Pyrethrins (Pyrethrin II)	12.1	373.1	161.1	133.2	+
65.	Spinetoram (Spinosyn L)	13.2	760.5	142.2	98.1	+
66.	Piperonyl butoxide-d9	13.2	365.4	177.4		+
67.	Piperonyl butoxide	13.3	356.3	177.2	119.2	+
68.	Chlorpyrifos	13.4	349.9	198.0	97.1	+
69.	Hexythiazox	13.7	353.1	228.1	168.1	+
70.	Etoxazole	14.6	360.2	141.1	304.2	+
71.	Spiromesifen	14.7	388.4	273.3	255.3	+
72.	Pyrethrins (Pyrethrin I)	15.1	329.2	161.2	133.2	+
73.	Cyfluthrin	15.3	451.1	191.2		+
74.	Cyfluthrin (qualifier)	15.3	453.1	193.2		+
75.	Cypermethrin	15.6	433.1	191.0	416.0	+
76.	(E)-Fenpyroximate	15.7	422.2	366.1	138.1	+
77.	Pyridaben	16.3	365.1	147.2	309.2	+
78.	Permethrin (trans)	16.6	408.3	183.2	355.1	+
79.	Permethrin (cis)	16.9	408.3	183.2	355.1	+
80.	Abamectin	16.9	890.5	305.4	567.4	+
81.	Etofenprox	17.0	394.3	177.2	359.3	+
82.	Bifenthrin-d6	17.1	446.3	181.3		+
83.	Bifenthrin	17.2	440.0	181.2	166.2	+
84.	Acequinocyl	18.2	402.3	343.2	189.0	+

Column

Raptor 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/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)

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

Water, 2 mM ammonium formate, 0.1% formic acid

Methanol, 2 mM ammonium formate, 0.1% formic acid

Time (min)	Flow (mL/min)	%A	%B
0.00	0.4	95	5
1.0	0.4	50	50
2.5	0.4	50	50
4.0	0.4	35	65
7.0	0.4	35	65
7.5	0.4	30	70
9.0	0.4	30	70
9.5	0.4	25	75
11.0	0.4	25	75
11.5	0.4	20	80
13.5	0.4	20	80
15.5	0.4	5	95
16.5	0.4	0	100
19.5	0.4	0	100
19.6	0.4	95	5

Detector	MS/MS
Ion Source:	Electrospray
Ion Mode:	ESI+/ESI-
Mode:	MRM
Instrument	Shimadzu Nexera X2
Sample Preparation	1 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.
Notes	Autosampler temperature: 10 °C

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