Cannabis sativa Species Overview

Experiment: MPGR

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Protocol for LC-TOF
LabPI	A. Daniel Jones
Analyst	Mary Dawn Celiz
LC system	Prominence High Performace Liquid Chromatograph
Manufacturer	Shimadzu
Degasser	DGU-20A5
Solvent Delivery	LC-20AD
System Controller	SCL-10AVP
Autosampler	SIL-50000
Column Oven	CTO-20A
Column	Ascentis® Express C18 Analytical HPLC column, 5 cm x 0.21 cm, 2.7 µm
Manufacturer of column	Supelco
Catalogue number	53822-U
Serial number	USMD003586
Packing Lot number	S10035
Injection volume	10 uL
Flow rate	0.3 mL/min
Mobile phases
A	0.5 mM ammonium acetate, pH 3.85
B	MeOH
Gradient Profile	Gradient program started with 1% B- 99% A, held for one minute, increased to 30% B in 1.5 minutes, then increased to 50% B in 5.5 minutes, further increase to 70% B in four minutes, followed by 99% B in ten minutes, held at 99 % B for four minutes, decrea
Column oven temperature	50?C
Sample temperature in the autosampler	10?C
Inlet method name	NIH_CAN_OPT_AscExp_004
Mass Spectrometer	Micromass? LCT PremierTM time-of-flight (TOF) mass spectrometer
Manufacturer	Waters
Software	MassLynxTM Version 4.1
Ionization source	Electrospray ionization (ESI)
Data acquisition	W mode, centroid
Polarity	Positive and Negative
Mass Range	50-1500 m/z
Aperture 1 voltage
Function 1	20 V
Function 2	40 V
Function 3	60 V
Function 4	80 V
MS method file	MDC_CAN_pos or MDC_CAN_neg
Manipulation of data
Lock mass	Telmisartan was used as lock mass standard.

Protocol for MarkerLynx
Function	1
Initial Retention Time (min)	0.3
Final Retention Time (min)	21
Low Mass	50
High Mass	1500
Mass Tolerance (Da)	0.05
Apex Track Peak Parameters
Peak Width at 5% Height (seconds)	automatic
Peak-to-Peak Baseline Noise	automatic
Apply smoothing	Yes
Collection Parameters
Marker Intensity threshold (counts)	20
Mass Window (Da)	0.05
Retention Time Window (min)	0.2
Noise Elimintation Level	10
Deisotope Data	Yes

Protocol for QuanLynx
Use absolute mass window	Yes
Chromatogram Mass Window (Da)	0.05
Response Type	External (absolute)
Response Uses	Area
Concentration of Standard (µM)	0.25, 0.5, 1, 2.5, 5, 10, 20
Retention Time Parameters
Locate Peak Using	Retention time
Retention Time Window (min) ±	0.2
Locate Peak Selection	Largest
Calibration Properties
Polynomial Type	Linear
Calibration Origin	Force
Weighing Function	1/X
Concentration Units	µM
Integration Properties
Smoothing Enabled	YES
Smooth Parameters
Smoothing Method	Mean
Smooting Iterations	1
Smoothing Width	2
Apex Track Enables	Yes
Apex Track Parameters
Peak-to-Peak Baseline Noise	Automatic
Peak width at 5% height	Automatic
Baseline Start Threshold %	0
Baseline End Threshold %	0.5

Sample Handling
Protocol when analyzing the samples	Before each batch of samples was analyzed, the mass spectrometer was calibrated using 0.1% phosphoric acid. After column equilibration, two methanol injections were performed first. Standard solutions were injected followed by a blank injection. After eve
Sample handling	Samples were received as dried extract. These were dissolved in 10 mL of 9:1 v/v methanol:chloroform, then sonicated. An aliquot of 500 uL was obtained from each extract and placed in polypropylene centrifuge tubes. These were dried in a SpeedVac Concentr
Sample storage temperature	Room temperature

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