California Cannabis Pesticides and Mycotoxins in Brownies on Raptor ARC-18 / Restek Searchable Chromatogram Library / Restek.com

	Peaks	t_R (min)	Precursor Ion	Product Ion 1	Product Ion 2	Polarity
1.	Daminozide-d6	0.6	167.0	149.3	49.3	+
2.	Daminozide	0.7	161.1	44.1	143.2	+
3.	Acephate	1.5	184.0	143.1	95.1	+
4.	Oxamyl	1.8	237.1	72.1	90.1	+
5.	Flonicamid	1.9	230.1	203.1	174.1	+
6.	Methomyl	1.9	163.1	88.1	106.1	+
7.	Thiamethoxam	1.9	292.0	211.1	181.1	+
8.	Imidacloprid	2.2	256.1	209.1	175.1	+
9.	Mevinphos I	2.2	225.1	127.1	193.2	+
10.	Acetamiprid	2.2	223.0	126.1	56.1	+
11.	Dimethoathe-d6	2.2	236.1	205.1	-	+
12.	Dimethoate	2.3	230.0	199.1	125.1	+
13.	Thiacloprid	2.4	253.0	126.0	90.1	+
14.	Mevinphos II	2.4	225.1	127.1	193.2	+
15.	Aflatoxin G2	2.4	331.2	189.3	115.2	+
16.	Aflatoxin G1	2.4	329.2	243.2	215.3	+
17.	Aldicarb	2.5	116.0	89.2	70.2	+
18.	Aflatoxin B2	2.5	315.3	287.2	243.3	+
19.	Dichlorvos	2.6	220.9	109.1	79.2	+
20.	Dichlorvos-d6	2.6	227.0	115.1	-	+
21.	Aflatoxin B1	2.6	313.2	241.2	128.2	+
22.	Imazalil	2.6	297.0	159.0	201.0	+
23.	Carbofuran	2.6	222.1	123.1	165.2	+
24.	Propoxur	2.6	210.1	111.1	93.1	+
25.	Carbaryl-d7	2.7	209.2	152.2	-	+
26.	Carbaryl	2.7	202.1	145.1	127.1	+
27.	Diuron-d6	2.9	239.1	78.2	-	+
28.	Atrazine-d5	2.9	221.2	179.1	-	+
29.	Naled	2.9	397.8	127.1	109.1	+
30.	Metalaxyl	2.9	280.2	220.2	192.2	+
31.	Spiroxamine	2.9	298.3	144.2	100.2	+
32.	Chlorantraniliprole	3.0	483.9	452.9	285.9	+
33.	Phosmet	3.0	318.0	160.1	77.2	+
34.	Azoxystrobin	3.1	404.0	372.1	344.1	+
35.	Linuron-d6	3.1	255.1	160.1	-	+
36.	Fludioxonil	3.2	247.0	180.0	126.0	-
37.	Methiocarb	3.2	226.1	169.1	121.1	+
38.	Dimethomorph I	3.2	388.2	301.2	165.3	+
39.	Boscalid	3.2	342.9	307.1	140.1	+
40.	Paclobutrazol	3.3	294.3	70.1	125.1	+
41.	Malathion	3.3	331.0	127.2	285.2	+
42.	Dimethomorph II	3.4	388.2	301.2	165.3	+
43.	Myclobutanil	3.4	289.1	70.1	125.1	+
44.	Bifenazate	3.4	301.0	198.1	170.2	+
45.	Ochratoxin A	3.5	404.2	239.1	358.3	+
46.	Fenhexamid	3.5	302.1	97.1	55.2	+
47.	Spirotetramat	3.7	374.2	302.1	216.1	+
48.	Ethoprophos	3.8	243.1	131.1	97.1	+
49.	Fipronil	3.8	436.8	331.8	251.9	-
50.	Fenoxycarb	3.9	302.1	88.1	116.1	+
51.	Kresoxim-methyl	4.1	314.2	267.2	222.2	+
52.	Tebuconazole	4.2	308.1	70.1	125.1	+
53.	Diazinon-d10	4.2	315.2	170.2	-	+
54.	Spinosyn A (spinosad)	4.3	732.4	142.2	98.1	+
55.	Diazinon	4.3	305.1	169.2	153.2	+
56.	Coumaphos	4.4	363.1	227.1	307.1	+
57.	Pyridaben	4.4	365.1	309.2	147.2	+
58.	Propiconazole	4.4	342.0	159.0	69.2	+
59.	Clofentezine	4.5	303.0	138.1	102.1	+
60.	Spinosyn D (spinosad)	4.8	746.5	142.3	98.4	+
61.	Spinosyn J (spinetoram)	4.8	748.5	142.3	98.3	+
62.	Trifloxystrobin	4.9	409.2	186.1	145.1	+
63.	Prallethrin	4.9	301.2	123.2	105.2	+
64.	Pyrethrin II	5.2	373.1	161.1	133.2	+
65.	Spinosyn L (spinetoram)	5.4	760.5	142.2	98.1	+
66.	Piperonyl butoxide	5.7	356.3	177.2	119.2	+
67.	Chlorpyrifos	5.8	349.9	198.0	97.1	+
68.	Hexythiazox	5.9	353.1	228.1	168.1	+
69.	Etoxazole	6.4	360.2	141.1	304.2	+
70.	Spiromesifen	6.4	273.2	255.2	187.2	+
71.	Pyrethrin I	6.6	329.2	161.2	105.2	+
72.	Cyfluthrin (qualifier)	6.6	453.1	193.2	-	+
73.	Cyfluthrin	6.6	451.1	191.2	-	+
74.	Cypermethrin	6.8	433.1	191.0	416.0	+
75.	Fenpyroximate	6.8	422.2	366.1	138.1	+
76.	trans-Permethrin	7.4	408.3	183.2	355.1	+
77.	cis-Permethrin	7.7	408.3	183.2	355.1	+
78.	Avermectin B1a	7.7	890.5	305.4	567.4	+
79.	Etofenprox	7.8	394.3	177.2	359.3	+
80.	Bifenthrin	8.0	440.0	181.2	166.2	+
81.	Acequinocyl (precursor ion 1)	9.3	402.3	343.2	189.0	+
82.	Acequinocyl (precursor ion 2)	9.3	386.0	344.2	189.1	+

LC_GN0602

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.:

5-15 ng/mL (Expected concentration range in extract of brownie initially spiked at 100 ng/g.)

Inj. Vol.:

2 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	0.5	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	0.5	95	5

Detector

MS/MS

Ion Mode:

ESI+/ESI-

Mode:

MRM

Instrument

UHPLC

Notes

Brownies 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.

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	California Pesticide Standards cat.# 34124 Qty:
	California Pesticide Standards cat.# 34125 Qty:
	California Pesticide Standards cat.# 34126 Qty:
	California Pesticide Standards cat.# 34127 Qty:
	California Pesticide Standards cat.# 34128 Qty:
	California Pesticide Standards cat.# 34129 Qty:
	Dimethoate-d6 Standard cat.# 31988 Qty:
	Dichlorvos-d6 Standard cat.# 31987 Qty:
	Carbaryl-d7 Standard cat.# 31985 Qty:
	Diazinon-d10 Standard cat.# 31986 Qty:
	Atrazine-d5 Standard cat.# 31984 Qty:
	Diuron-d6 Standard cat.# 31989 Qty:
	Linuron-d6 Standard cat.# 31990 Qty:
	Aflatoxins (B1, B2, G1, G2) Standard cat.# 34121 Qty:
	Ochratoxin A Standard cat.# 34122 Qty:
	Raptor EXP Guard Column Cartridges cat.# 9314A0252 Qty:
	Raptor ARC-18 LC Columns cat.# 9314A12 Qty:
	Resprep SPE Cartridges cat.# 26030 Qty:

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