# Dataset title

PCB method design of experiments

# Dataset authors

- Porru, Emanuele	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0001-8041-1085
- Comito, Rossana	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0009-0008-3085-7167
- Kassouf, Nicholas	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0002-0930-6378
- Zappi, Alessandro	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0002-0029-4403
- Interino, Nicolò	IRCCS Institute of Neurological Sciences of Bologna, 40139 Bologna, Italy	https://orcid.org/0000-0002-7302-1246
- Fiori, Jessica	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0002-6004-5118
- Melucci, Dora	    Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0001-5505-6763
- Violante, Francesco Saverio	Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy	https://orcid.org/0000-0003-4084-2782

# Contributors

- Comito, Rossana   Alma Mater Studiorum, University of Bologna, 40138 Bologna, Italy https://orcid.org/0009-0008-3085-7167 Data collector
- Porru, Emanuele   Contact person

# Dates

Dataset submitted on November 2025.

# License

This dataset is released under a Creative Commons Attribution 4.0 (CC BY 4.0) License, https://creativecommons.org/licenses/by/4.0/

# Abstract

This dataset contains the complete experimental matrices and multivariate responses used for the optimization of Gas Chromatography-Mass Spectrometry (GC–MS) analytical conditions and extraction procedures in the simultaneous determination of Polychlorinated biphenyl (PCB), brominated flame retardants (BFR) and novel brominated flame retardants (NBFR) in human serum. Four CSV files are provided. DesignOfExperiment_RF_LOQ.csv reports the D-optimal and full-factorial experimental designs used to optimize retention factor (RF), chromatographic separation, and limit of quantification (LOQ), including variable levels for injection parameters, oven temperatures, and pulse conditions. DesignOfExperiment_extraction.csv contains the extraction-optimization DoE evaluating the effect of hexane and ethyl acetate volumes and SPE elution composition on analyte recovery and matrix effects. PrincipalComponentAnalysis_RF_LOQ.csv includes A/FWHM ratios for all target analytes, used to compute Principal Component Analysis (PCA) models that summarize global chromatographic performance during method refinement. PrincipalComponentAnalysis_extraction.csv provides recovery-based PCA input data for assessing extraction efficiency across pollutant classes. Together, these datasets support full reproducibility of the chemometric workflow applied in the associated study, enabling reconstruction of DoE models, PCA analyses, and optimization paths. Typical uses include method-development benchmarking, teaching of multivariate optimization strategies, and re-analysis of GC–MS development data under alternative criteria.

# Dataset documentation

This folder contains datasets related to the optimization of retention factor (RF), limit of quantification (LOQ) and extraction of several polluttants in Gas-Chromatography coupled with mass spectrometry. Each file corresponds to a specific experimental design (DoE) or principal component analysis (PCA) used in the study.
All datasets are provided as CSV files.

## file: designOfExperiments_RF_LOQ.csv

*Content: Experimental design data for Retention Factor(RF) and Limit of Quantification (LOQ) optimization.

AL1-AL64: First retention time optimization
A 1-64: number of experiments
B 1-64: level of variable "Sampling time (°C/min)"
C 1-64: level of variable "Temperature 2 (°C)
D 1-64: level of variable "Time (min)"
E 1-64: level of variable "Sampling time 2(°C/min)"
F 1-64: level of variable "Final Temperature (°C)"
G 1-64: level of variable "Final time (min)"
H 1-64: level of variable "Pulse Pressure (Psi)"
I 1-64: level of variable "Time of Pulse Pressure (min)"
J 1-64: level of variable "Purge flow (mL/min)"
K 1-64: level of variable "Purge time (min)"
L 1-64: Response (Retention Factor)
										
AG68- AG105: Second retention factor optimization:
A 69-105: number of experiments
B 69-105: level of variable "Temperature 2 (°C)
C 69-105: level of variable "Time (min)"
D 69-105: level of variable "Sampling time 2(°C/min)"
E 69-105: level of variable "Pulse Pressure (Psi)"
F 69-105: level of variable "Time of Pulse Pressure (min)"
G 69-105: Response (Retention Factor)

AL108- AL171: First Limit of quantification optimization
A 108-171: number of experiments
B 108-171: level of variable "Sampling time (°C/min)"
C 108-171: level of variable "Temperature 2 (°C)
D 108-171: level of variable "Time (min)"
E 108-171: level of variable "Sampling time 2(°C/min)"
F 108-171: level of variable "Final Temperature (°C)"
G 108-171: level of variable "Final time (min)"
H 108-171: level of variable "Pulse Pressure (Psi)"
I 108-171: level of variable "Time of Pulse Pressure (min)"
J 108-171: level of variable "Purge flow (mL/min)"
K 108-171: level of variable "Purge time (min)"
L 108-171: Response (Score on PC1)

AG175- AG212: Second limit of quantification optimization:
A 175-212: number of experiments
B 175-212: level of variable "Temperature 2 (°C)
C 175-212: level of variable "Time (min)"
D 175-212: level of variable "Sampling time 2(°C/min)"
E 175-212: level of variable "Pulse Pressure (Psi)"
F 175-212: level of variable "Time of Pulse Pressure (min)"
G 175-212: Response (Retention Factor)

## file: PrincipalComponentAnalysis_RF_LOQ.csv

*Content: each column contains the ratio of the peak area to the full width at half maximum used for Principal Component Analysis
AAX1-AAX63: Principal component analysis related to the first experimental design
A 1-63: number of experiments
B 1-63: 2,4,6,tribrphenol	
C 1-63: Atrazina 	
D 1-63: Allyl 2,4,5-tribrphenyl_ether	
E 1-63: 3cl-pcb(18) 	
F 1-63: 3cl-pcb(31)
G 1-63: 3cl-pcb(28)	
H 1-63: alachlor	 
I 1-63: 4cl-pcb(52) 	
J 1-63: 4cl-pcb(44) 	
K 1-63: 5cl-pcb(95) 	
L 1-63: 5cl-pcb(101) 	
M 1-63: 5cl-pcb(99)
N 1-63: Tetrabr-o-cl-toluene 	
O 1-63: 4cl-pcb81	
P 1-63: 1,2,3,4,5-Pentabromo-6-chlorocyclohexane	
Q 1-63: 4cl-pcb77	 
R 1-63: 5cl-pcb110	
S 1-63: 6cl-pcb(151)  
T 1-63: 5cl-pcb(123) 		 	 
U 1-63: 6cl-pcb(149) 	
V 1-63: 5cl-pcb(118) 	
W 1-63: PentaBr_toluene 	
X 1-63: 5cl-pcb(114)	
Y 1-63: 6cl-pcb(146)	 
Z 1-63: 6cl-pcb(153)	  
AA 1-63: 5cl-pcb(105)	 
AB 1-63: 6cl-pcb(138)	 
AC 1-63: 5cl-pcb(126)	
AD 1-63: 7cl-pcb(187)  
AE 1-63: 7cl-pcb(180) 	
AF 1-63: 6cl-pcb(128)	
AG 1-63: 6cl-pcb(167)	 
AH 1-63: TetraBR_phtalic_anydride	  
AI 1-63: HexaBR_benzene	 
AJ 1-63: 7cl-pcb(183)	 
AK 1-63: 6cl-pcb(156)	
AL 1-63: 6cl-pcb(157)	  
AM 1-63: 7cl-pcb(177)	  
AN 1-63: TetraBR_diphenyl_ether 
AO 1-63: 6cl-pcb(169) 	 
AP 1-63: 7cl-pcb(170)	
AQ 1-63: 7cl-pcb(189)  

AAS66-AAS103: principal component analysis related to the second experimental design
A 66-103: number of experiments
B 66-103: 2,4,6,tribrphenol	
C 66-103: Allyl 2,4,5-tribrphenyl_ether	
D 66-103: 3cl-pcb(18) 	
E 66-103: 3cl-pcb(31)
F 66-103: 3cl-pcb(28)		 
G 66-103: 4cl-pcb(52) 	
H 66-103: 4cl-pcb(44) 
I 66-103: 5cl-pcb(95) 	
J 66-103: 5cl-pcb(101) 	
K 66-103: 5cl-pcb(99)
L 66-103: Tetrabr-o-cl-toluene 	
M 66-103: 4cl-pcb81		
N 66-103: 4cl-pcb77	 
O 66-103: 5cl-pcb110	
P 66-103: 6cl-pcb(151)  
Q 66-103: 5cl-pcb(123) 		 	 
R 66-103: 6cl-pcb(149) 	
S 66-103: 5cl-pcb(118) 	
T 66-103: PentaBr_toluene 	
U 66-103: 5cl-pcb(114)	
V 66-103: 6cl-pcb(146)	 
W 66-103: 6cl-pcb(153)	  
X 66-103: 5cl-pcb(105)
Y 66-103: 6cl-pcb(138)
Z 66-103: 5cl-pcb(126)	 
AA 66-103: 7cl-pcb(187)	 
AB 66-103: 7cl-pcb(180) 	
AV 66-103: 6cl-pcb(128)	  
AD 66-103: 6cl-pcb(167) 	
AE 66-103: HexaBR_benzene
AF 66-103: 7cl-pcb(183)	 
AG 66-103: 6cl-pcb(156)		 
AH 66-103: 6cl-pcb(157)		 
AI 66-103: 7cl-pcb(177)
AJ 66-103: TetraBR_diphenyl_ether  
AK 66-103: 6cl-pcb(169)	  
AL 66-103: 7cl-pcb(170) 
AM 66-103: 7cl-pcb(189)  	 
AN 1-63: PentaBR_benzyl_acrilate 	
AO 1-63: 2,2-Bis(4-allyloxy-3,5-dibromophenyl)propane 
AP 1-63: 2ethylexyx_tetrabr_benzoate 
AQ 1-63: HexaBRCyclododecane  
AR 1-63: 1,2-bis (2,4,6-tribromophenoxy)ethane   
AS 1-63: Bis (2-ethylhexyl)-3,4,5,6-tetrabromo-phthalate  

# file: PrincipalComponentAnalysis_extraction.csv

*Content: each column contains the recovery of the pollutants obtained in the extraction method development and used for the principal component analysis. 
A 2-24: number of experiments
B 2-24: 2,4,6,tribrphenol	
C 2-24: Allyl 2,4,5-tribrphenyl_ether	
D 2-24: 3cl-pcb(18) 	
E 2-24: 3cl-pcb(31)
F 2-24: 3cl-pcb(28)		 
G 2-24: 4cl-pcb(52) 	
H 2-24: 4cl-pcb(44) 
I 2-24: 5cl-pcb(95) 	
J 2-24: 5cl-pcb(101) 	
K 2-24: 5cl-pcb(99)
L 2-24: Tetrabr-o-cl-toluene 	
M 2-24: 4cl-pcb81		
N 2-24: 4cl-pcb77	 
O 2-24: 5cl-pcb110	
P 2-24: 6cl-pcb(151)  
Q 2-24: 5cl-pcb(123) 		 	 
R 2-24: 6cl-pcb(149) 	
S 2-24: 5cl-pcb(118) 	
T 2-24: PentaBr_toluene 	
U 2-24: 5cl-pcb(114)	
V 2-24: 6cl-pcb(146)	 
W 2-24: 6cl-pcb(153)	  
X 2-24: 5cl-pcb(105)
Y 2-24: 6cl-pcb(138)
Z 2-24: 5cl-pcb(126)	 
AA 2-24: 7cl-pcb(187)	 
AB 2-24: 7cl-pcb(180) 	
AV 2-24: 6cl-pcb(128)	  
AD 2-24: 6cl-pcb(167) 	
AE 2-24: HexaBR_benzene
AF 2-24: 7cl-pcb(183)	 
AG 2-24: 6cl-pcb(156)		 
AH 2-24: 6cl-pcb(157)		 
AI 2-24: 7cl-pcb(177)
AJ 2-24: TetraBR_diphenyl_ether  
AK 2-24: 6cl-pcb(169)	  
AL 2-24: 7cl-pcb(170) 
AM 2-24: 7cl-pcb(189)  	 
AN 2-24: PentaBR_benzyl_acrilate 	
AO 2-24: 2,2-Bis(4-allyloxy-3,5-dibromophenyl)propane 
AP 2-24: 2ethylexyx_tetrabr_benzoate 
AQ 2-24: HexaBRCyclododecane  
AR 2-24: 1,2-bis (2,4,6-tribromophenoxy)ethane   
AS 2-24: Bis (2-ethylhexyl)-3,4,5,6-tetrabromo-phthalate  

# file: DesignOfExperiment_extraction.csv

*Content: experiments matrix used for design of experiments model
A2-20: Experiments number
B2-20: Hexane
C2-20: Ethyl acetate
D2-20: Dichloromethane

# File specifications

CSV files use Windows 1252 (Western Europe) character encoding. Semicolon (;) is used as field separator.