Dear Bryan,

The following is a procedure to determine phenolic compounds found in wastewater by GC-MS analysis:

Methodology

(1) Identification and quantification of phenolic compounds. There are 3 steps to identify phenolic compounds in water: 1) sample preparation; 2) determination by GC-MS; and 3) analysis, based on the library of silylated phenolic compounds,

using RTL, GC-MS ChemStation and DRS. After preparing the samples by the optimized method, the samples were analyzed using GC-MS in scan and selected

ion monitoring (SIM) mode using the RTL method. The scan data were analyzed using DRS to identify the compounds in the sample matrices. Combined spectra of samples were analyzed by GC-MS with the library of silylated phenolic compounds, and a contaminant list including all the phenolic compounds was identified using spectral deconvolution technology. The phenolic compounds identified by GC-MS were quantified using the SIM results. (2) Criteria for selecting target phenolic compounds. The selection of 50 target phenolic compounds was based on following criteria: 1) wide use (the production or requirement or import and export amount of one phenolic compound exceeded 1000 t y–1); 2) availability of relevant

toxicity data; and 3) availability of a standard. (3) Procedures for building library. After derivatized by BSTFA with 1% TMCS, each standard compound was analyzed

by GC-MS to obtain their mass spectrogram. A library of silylated phenolic compounds was created as a .tab file using Microsoft Excel in which compound name, retention time, target ion, quota ion and abundance ratio of ion of

each target compound were recorded. A series of conversions were then carried out to build the library. Details for establishing a library can be found in the Agilent Technical Overview [14]. (4) Optimizing the preparation method. To prepare artificial

samples in the laboratory, Milli-Q water samples of 2 L were spiked by adding a mixture of phenolic compounds (including 12 phenolic compounds) dissolved in

methanol to obtain a concentration of 250 ng L–1 for each analyte. All artificial samples were adjusted to pH < 2 with 6 μmol L–1 hydrochloride buffer, filtered through Millipore glass microfiber filters, preserved in brown glass containers,

and processed by solid-phase extraction within 2 d. Samples were enriched by SPE using the C18 cartridge, the HLB cartridge and the C18 cartridge coupled with the HLB cartridge. For the recovery test, a total of 12 different solvents were tested. Matrix spiked experiments were used to validate the selected optimized elution solvents. Derivatization was performed to reduce the polarity of phenolic compounds. All extracts were evaporated under a gentle stream of nitrogen. The dry residues were derivatized by 100 μL BSTFA with 1% TMCS and heated in a heating block at 60°C for 2 h [15]. TMCS can enhance the chemical reactivity of silylating agents. The derivatives were cooled to room temperature and then dissolved with 400 μL n-hexane to yield the sample solution. The constant volume

of solutions was 500 μL.

This procedure was taken from:

A gas chromatography/mass spectrometry method for the simultaneous analysis of 50 phenols in wastewater using deconvolution technology

ZHONG WenJue1 , WANG DongHong1 , XU XiaoWei1 , WANG BingYi1 , LUO Qian1 , SENTHIL KUMARAN Satyanarayanan2 & WANG ZiJian1*

Environmental Chemistry January 2011 Vol.56 No.3: 275–284

http://download.springer.com/static/pdf/541/art%253A10.1007%252Fs11434-010-4266-1.pdf?originUrl=http%3A%2F%2Flink.springer.com%2Farticle%2F10.1007%2Fs11434-010-4266-1&token2=exp=1466364317~acl=%2Fstatic%2Fpdf%2F541%2Fart%25253A10.1007%25252Fs11434-010-4266-1.pdf%3ForiginUrl%3Dhttp%253A%252F%252Flink.springer.com%252Farticle%252F10.1007%252Fs11434-010-4266-1*~hmac=af655475349c111dfdac2520bcbe4d6cb276f52fe73223c2feb2ef143d290cb9

Hoping this will be helpful,

Rafik

Dear Bryan,

The following is a procedure to determine phenolic compounds found in wastewater by GC-MS analysis:

Methodology

(1) Identification and quantification of phenolic compounds. There are 3 steps to identify phenolic compounds in water: 1) sample preparation; 2) determination by GC-MS; and 3) analysis, based on the library of silylated phenolic compounds,

using RTL, GC-MS ChemStation and DRS. After preparing the samples by the optimized method, the samples were analyzed using GC-MS in scan and selected

ion monitoring (SIM) mode using the RTL method. The scan data were analyzed using DRS to identify the compounds in the sample matrices. Combined spectra of samples were analyzed by GC-MS with the library of silylated phenolic compounds, and a contaminant list including all the phenolic compounds was identified using spectral deconvolution technology. The phenolic compounds identified by GC-MS were quantified using the SIM results. (2) Criteria for selecting target phenolic compounds. The selection of 50 target phenolic compounds was based on following criteria: 1) wide use (the production or requirement or import and export amount of one phenolic compound exceeded 1000 t y–1); 2) availability of relevant

toxicity data; and 3) availability of a standard. (3) Procedures for building library. After derivatized by BSTFA with 1% TMCS, each standard compound was analyzed

by GC-MS to obtain their mass spectrogram. A library of silylated phenolic compounds was created as a .tab file using Microsoft Excel in which compound name, retention time, target ion, quota ion and abundance ratio of ion of

each target compound were recorded. A series of conversions were then carried out to build the library. Details for establishing a library can be found in the Agilent Technical Overview [14]. (4) Optimizing the preparation method. To prepare artificial

samples in the laboratory, Milli-Q water samples of 2 L were spiked by adding a mixture of phenolic compounds (including 12 phenolic compounds) dissolved in

methanol to obtain a concentration of 250 ng L–1 for each analyte. All artificial samples were adjusted to pH < 2 with 6 μmol L–1 hydrochloride buffer, filtered through Millipore glass microfiber filters, preserved in brown glass containers,

and processed by solid-phase extraction within 2 d. Samples were enriched by SPE using the C18 cartridge, the HLB cartridge and the C18 cartridge coupled with the HLB cartridge. For the recovery test, a total of 12 different solvents were tested. Matrix spiked experiments were used to validate the selected optimized elution solvents. Derivatization was performed to reduce the polarity of phenolic compounds. All extracts were evaporated under a gentle stream of nitrogen. The dry residues were derivatized by 100 μL BSTFA with 1% TMCS and heated in a heating block at 60°C for 2 h [15]. TMCS can enhance the chemical reactivity of silylating agents. The derivatives were cooled to room temperature and then dissolved with 400 μL n-hexane to yield the sample solution. The constant volume

of solutions was 500 μL.

This procedure was taken from:

A gas chromatography/mass spectrometry method for the simultaneous analysis of 50 phenols in wastewater using deconvolution technology

ZHONG WenJue1 , WANG DongHong1 , XU XiaoWei1 , WANG BingYi1 , LUO Qian1 , SENTHIL KUMARAN Satyanarayanan2 & WANG ZiJian1*

Environmental Chemistry January 2011 Vol.56 No.3: 275–284

http://download.springer.com/static/pdf/541/art%253A10.1007%252Fs11434-010-4266-1.pdf?originUrl=http%3A%2F%2Flink.springer.com%2Farticle%2F10.1007%2Fs11434-010-4266-1&token2=exp=1466364317~acl=%2Fstatic%2Fpdf%2F541%2Fart%25253A10.1007%25252Fs11434-010-4266-1.pdf%3ForiginUrl%3Dhttp%253A%252F%252Flink.springer.com%252Farticle%252F10.1007%252Fs11434-010-4266-1*~hmac=af655475349c111dfdac2520bcbe4d6cb276f52fe73223c2feb2ef143d290cb9

Hoping this will be helpful,

Rafik

Try using LCMS-QToF

See USEPA method 625. Most of the published methods are based on the USEPA procedure.

Check this method:

Article Application of dispersive liquid-liquid microextraction and ...

regards,

G

dear colleague, do derivatization using BSTFA to your sample (make your compounds more volatile) then do a GC-MS.

best regards.