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GC Analysis of Tetrahydrocannabinol (THC) and Carboxytetrahydrocannabinol (THCCOOH) in Surface Water on SLB®-5ms after SPME using 50/30 μm DVB/Carboxen/PDMS Fiber, On-Fiber Derivatization

GC Analysis of Tetrahydrocannabinol (THC) and Carboxytetrahydrocannabinol (THCCOOH) in Surface Water on SLB®-5ms after SPME using 50/30 μm DVB/Carboxen/PDMS Fiber, On-Fiber Derivatization suitable for GC, application for SPME

材料

SPME 光纤

产品编号
说明
价格

57348-U

SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS)

needle size 24 ga, StableFlex

分析色谱柱

产品编号
说明
价格

28564-U

SLB ®-5 ms 毛细管 GC 色谱柱

L × I.D. 20 m × 0.18 mm, df 0.18 μm

标准

产品编号
说明
价格

T-003

−-Δ9-四氢大麻酚-D3标准液 溶液

100 μg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

T-004

(±)-11-nor-9-羧基-Δ9-四氢大麻酚-D3标准液 CRM 溶液

100 μg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

T-005

(−)-Δ9-四氢大麻酚标准液 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

T-006

(±)-Δ-四氢大麻酸标准液 溶液

100 μg/mL in methanol, ampule of 1 mL, Cerilliant®

试剂

产品编号
说明
价格

69479

N-甲基-N-（三甲基硅烷基）三氟乙酰胺

for GC derivatization, LiChropur™, ≥98.5%

配件

产品编号
说明
价格

2637501

进样口衬管，直接 (SPME) 型，直型设计（未包装）

pkg of 1 ea

SU860099

顶空瓶，螺旋盖，圆底（仅小瓶），100个装

volume 10 mL, clear glass vial, thread for 18, O.D. × H 22.5 mm × 46 mm, pkg of 100 ea

SU860101

顶空样品瓶的磁性螺旋盖，18 mm螺纹，1.5mm隔垫，100个装

PTFE/silicone septum (white PTFE/tranparent blue silicone), septum thickness 1.3 mm, pkg of 100 ea

CONDITIONS

sample preparation

SPME

sample/matrix

8 mL surface water in 10 mL vial, adjusted to pH 2 with HCl, spiked with THC and THCCOOH at 50 ng/L each compound

SPME fiber

StableFlex™ SPME Fiber, DVB/CARBOXEN-PDMS, 2 cm

extraction

immersion, 60 min, 60 °C

desorption process

260° C, 3 min

sample preparation

post-extraction derivatization: 500 μL MSTFA in 10 mL vial, headspace, 30 min, 60 °C

sample preparation

fiber post-bake: 10 min, 270 °C

column

SLB-5ms: 20 m x 0.18 mm I.D., 0.18 μm (28564-U)

oven

90°C (3 min), 20 °C/min to 200 °C, 3 °C/min to 300°C (5 min)

inj. temp.

260 °C

detector

MSD

MSD interface

325 °C

scan range

SIM:THC: m/z=303, 371(quant), 386;THCCOOH: m/z=371 (quant), 473, 488

carrier gas

helium, 1 mL/min constant flow

injection

splitless

liner

0.75 mm SPME

说明

分析说明

Cannabis is a Schedule 1 substance under US federal law. However, at the time of this writing, four US states have legalized it for recreational and medical use. The level of use by the general public is typically determined through questionnaires and crime statistics, but this approach may not give an accurate assessment. Sewage epidemiology seeks to correlate data from these surveys with actual levels found in wastewater. In the case of cannabis, this can be done by analyzing for the psychoactive substance, tetrahydrocannabinol (THC), and its major metabolite, carboxytetrahydrocannabinol (THCCOOH). THC can be analyzed by GC directly, but because THCCOOH contains an acid group in its structure it requires derivatization. Thus, if the two compounds are analyzed together, derivatization must be used. In this application, solid phase microextraction (SPME) with post-extraction, on-fiber derivatization was used for low level analysis of THC and THCCOOH from surface water prior to separation on an SLB®-5ms GC column. Cerilliant CRMs provided reliable quantification.

法律信息

SLB is a registered trademark of Merck KGaA, Darmstadt, Germany
StableFlex is a trademark of Sigma-Aldrich Co. LLC

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HPLC ColumnsGC Columns & AccessoriesTLC Plates & AdsorbentsSolid Phase Microextraction (SPME)Solid Phase Extraction & QuEChERS

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