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Zilfidou, E.; Kabir, A.; Furton, K.G.; Samanidou, V. Applications of Fabric Phase Sorptive Extraction. Encyclopedia. Available online: https://encyclopedia.pub/entry/46886 (accessed on 03 July 2024).
Zilfidou E, Kabir A, Furton KG, Samanidou V. Applications of Fabric Phase Sorptive Extraction. Encyclopedia. Available at: https://encyclopedia.pub/entry/46886. Accessed July 03, 2024.
Zilfidou, Eirini, Abuzar Kabir, Kenneth G. Furton, Victoria Samanidou. "Applications of Fabric Phase Sorptive Extraction" Encyclopedia, https://encyclopedia.pub/entry/46886 (accessed July 03, 2024).
Zilfidou, E., Kabir, A., Furton, K.G., & Samanidou, V. (2023, July 17). Applications of Fabric Phase Sorptive Extraction. In Encyclopedia. https://encyclopedia.pub/entry/46886
Zilfidou, Eirini, et al. "Applications of Fabric Phase Sorptive Extraction." Encyclopedia. Web. 17 July, 2023.
Applications of Fabric Phase Sorptive Extraction
Edit

Fabric phase sorptive extraction (FPSE) is a novel and green sample preparation technique introduced in 2014. FPSE utilizes a natural or synthetic permeable and flexible fabric substrate chemically coated with a sol-gel organic-inorganic hybrid sorbent in the form of ultra-thin coating, which leads to a fast and sensitive micro-extraction device. The flexible FPSE requires no modification of samples and allows direct extraction of analytes. Sol-gel sorbent-coated FPSE media possesses high chemical, solvent, and thermal stability due to the strong covalent bonding between the substrate and the sol-gel sorbent.

fabric phase sorptive extraction sample preparation chromatography applications microextraction green analytical chemistry

1. Introduction

It is well known that sample preparation is a very important and inevitable step in the chemical analysis workflow. Most of the real-life analytical samples cannot be directly analyzed with an injection into the analytical instrument. Furthermore, they have to be treated in a way that makes them compatible with the analytical instrument. Additionally, their collection and preparation require more than 80% of the analytical process time. As such, sample preparation is considered to be the most time-consuming but critical part of the whole analysis, which affects its effectiveness and performance. Therefore, the main purposes are the reduction of the matrix complexity and the separation and pre-concentration of the target analytes from the sample matrices in order to be ready for their introduction into the analytical instrument for identification and quantification [1][2].
As time passed, low-cost, fast, and environmentally-friendly procedures become necessary in order to improve quality of life and protect the environment. Scientists try to develop new analytical methodologies compliant with the principles of green analytical chemistry (GAC) [3]. Therefore, the classic sample preparation technique of liquid-liquid extraction (LLE) is replaced by solid-phase extraction (SPE), which has been widely accepted because of the simplicity of the device, the efficiency, the rapid separation process, the ability to extract polar compounds, no requirement of phase separation, and the lower organic solvent consumption [4]. To further minimize the amount of sample and solvent waste during the sample preparation step, to overcome some drawbacks of SPE is a multi-step procedure such as the requirement of solvent evaporation and sample reconstitution. Novel sorbent based micro-extraction techniques have been developed such as solid-phase micro-extraction (SPME) by Pawliszyn and co-workers in 1990, stir-bar sorptive extraction (SBSE) in 1999, magnetic solid-phase extraction technique (MSPE) in 1999, and micro-extraction in a packed syringe (MEPS) in 2004 [4][5].
It is estimated that the major drawbacks of most of the micro-extraction techniques are due to the primary contact surface area (PCSA) of the device and the coating technology that is applied to immobilize the sorbent on the substrate surface [2]. The PCSA is part of the surface area of the extraction media, which can be available for direct interaction with the analytes during the process. The augmentation in PCSA offers higher sorbent loading without any change in the coating technology. Therefore, more target analytes are adsorbed by the sorbent and reduction of the extraction equilibrium time is achieved. Additionally, the sorbent coating technology is very important. From all the alternative ones that have been developed, the sol-gel coating technology, proposed by Malik and co-workers, is the most flexible and convenient. There is a strong chemical bond between the sol-gel coated sorbent and the substrate, which leads to high solvent and chemical stability. Due to its inherent porosity, reduction of the extraction equilibrium time, and higher or equivalent sensitivity is achieved when compared to commercial SPME fibers. In summary, both the coating technology and the PCSA have to be increased, which results in a sensitive and fast sample preparation technique [6][7].
Based on these observations and developments, Kabir and Furton proposed a new, green sample preparation technique in 2014 called fabric phase sorptive extraction (FPSE). FPSE utilizes a natural or synthetic fabric substrate, which is chemically coated in the form of ultra-thin coating with sol-gel organic-inorganic hybrid sorbent as the extraction medium. Generally, the FPSE procedure consists of the following steps: first, the sol-gel sorbent coated FPSE media is submerged into a mixture of appropriate solvents to clean any undesirable impurities from the material and then it is rinsed with deionized water to remove the residues of organic solvents. Afterward, an amount of sample solution is transferred into a glass tube vial that contains a clean Teflon-coated magnetic stir bar inside and the FPSE media is introduced into the vial. The sample is magnetically stirred for an optimum extraction time where the sorption of the target analytes by the sorbent takes place. Subsequently, the FPSE device is removed from the vial and is brought in contact with the eluting solvent into another vial where desorption occurs and the retained analytes are back-extracted to this eluting system. Afterwards, the extract is centrifuged and filtered before being injected into the analytical instrument. The FPSE process is described schematically in Figure 1 [6][8][9]. The FPSE media can be reused for further extraction procedures by washing with a suitable solvent system and drying on a watch glass so that it can be ready for storage in an air-tight glass container for future use.
Figure 1. General presentation of fabric phase sorptive extraction.
The FPSE combines the extraction mode of SPME/SPE into a single technology platform. At the beginning of the whole procedure, the FPSE media is in contact with the sample or the aqueous solution along with the analytes of interest whose mass transfers the sorbent until an equilibrium between the sorbent and the sample matrix is established, which mimics the direct-immersion SPME (equilibrium extraction mode). The extraction process can be facilitated with magnetic stirring, sonication, and more. The porous network of sol-gel sorbent coating and the permeability of the substrate lead to the existing flow-through system, which mimics the solid phase extraction (exhaustive extraction mode) [7][10]. The fabric substrates that are used can be hydrophilic (cotton cellulose), hydrophobic (polyester), or both (cotton-polyester). The different nature of the substrates is very important and determines the selectivity and the polarity of the FPSE media. The strong chemical bonding between permeable fabric and porous sol-gel sorbent offers high chemical and solvent stability. Therefore, the FPSE device is reusable and can be exposed to any organic solvent or harsh chemical environment, which keeps its sorption capability unaffected. Additionally, it provides a high primary contact surface area (PCSA) for rapid analyte-sorbent interaction and, as a result, for rapid and efficient analyte extraction (fast extraction equilibrium). The flexible FPSE requires no modified samples but provides extraction of analytes directly from the sample matrices. Therefore, it eliminates any prior and post sample preparation procedure like filtration, centrifugation, solvent evaporation, and sample reconstitution, which avoids the risk of potential analyte loss, experimental errors, and sample preparation costs. A remarkable benefit of this two-step micro-extraction technique is the variety of the available sorbents that allows the application of the FPSE device in different kind of samples. Therefore, this simple, fast, and sensitive sample preparation technique can be successfully applied in environmental samples, biological samples, or food products [2][8][9][10][11][12]. Taking into account all the reported FPSE methods in the literature so far, it is concluded that the majority of them (57.14%) was applied to environmental samples while applications to food samples (25%) and finally to biological samples (17.86%) follow. All FPSE techniques reported in the literature and studied in the present entry are presented in Table 1 and classified according to the three sample categories in which they were applied. Experimental information of the FPSE methods, the target analytes, the samples, and the main analytical parameters obtained were included.
Table 1. Classification of the applications of the FPSE technique.

Analytical Technique

Fabric Substrate

Sol-Gel Coating

E.T. (min)

Elution System

Sample

Type of Analyte

Analyte

E.F.

LOD ng/L

LOQ ng/L

R%

Ref.

Environmental Samples

FPSE-HPLC-UV

Cellulose

PEG

40

MeOH-ACN

Tap-Pond-Reclaimed water

Substituted phenols

4-CP

-

30

-

91.0–109.5

[2]

3,5-DMP

10

73.2–90.7

2,6-DCP

40

19.7–40.7

2,4,6-TCP

20

26.9–57.0

2,4-DIPP

20

35.8–90.8

FPSE-HPLC-UV

Cellulose

PTHF

25

MeOH

Ground-River water, WWTP, Soil, Sludge

Alkylphenols

4-TBP

-

182

601

90.1–96.0

[13]

4-SBP

179

599

90.6–96.3

4-TAP

192

640

89.0–96.5

4-CP

161

531

91.1–96.9

FPSE-HPLC-FLD

Cellulose

PTHF

20

MeOH

Ground-River-Drinking, WWTP, Hospital wastewater

Estrogens

BPA

13.9

42

139

88.7–96.4

[12]

E2

14.4

20

66

89.4–97.4

EE2

14.7

36

119

89.0–98.0

FPSE-UHPLC-MS/MS

Cellulose

PTHF

20

MeOH

WWTP, Untreated Hospital wastewater, Tap water

Steroid hormones: Androgens Progestogens

NORET

-

33.5

-

79.3–95.4

[14]

NOR

1.7

79.5–103.5

MGA

21.4

102.2–121.2

PRO

6.9

79.8–96.9

BOL

46.9

66.6–92.4

NAN

50.7

82.2–102.4

TES

2.2

75.6–91.8

DHEA

264

77.6–92.7

AND

63.6

70.0–98.9

ADTD

19.4

65.9–97.8

FPSE-HS-GC-MS

Fiber glass

PDMDPS

-

He

Environmental air

Sexual pheromone

(3E,8Z,11Z)-

-

1.6 μg

5.3 μg

-

[15]

tetradecatrien-1-yl

   

acetate

   

(3E,8Z)-

0.8 μg

2.6 μg

tetradecadien-1-yl

   

acetate

   

FPSE-HPLC-UV

Cellulose

PTHF

20

ACN

Industrial-Ground water, Borcher-Oakay alloy

Heavy metal ions

Co(II)

-

20

66

89.6–98.7

[16]

Ni(II)

18

59

87.0–98.6

Pd(II)

10

30

89.0–99.0

       

FPSE-HPLC-UV

Cellulose

PTHF

15

ACN

Industrial-Bore well-Drinking water

Heavy metal ions

Cr(III)

-

1

3

89.6–98.7

[17]

Cr(IV)

3

9

87.0–98.6

       

FDSE-FI-FAAS

Polyester

PDMDPS

1.5

MIBK

River-Coastal-Ditch water

Toxic metals

Lead

140

1800

6000

95.0–101.0

[18]

Cadmium

38

400

1200

94.0–98.0

FPSE-UHPLC-MS/MS

Polyester

PDMDPS

60

MeOH

Sewage water

UV stabilizers in personal care products

UV P

10

12.8–25.3

42.7–84.3

83–99

[19]

UV 329

12.2–19.8

40.7–66.0

51–65

UV 326

51.6–60.7

172–202

49–65

UV 328

9.44–18.1

31.5–60.3

43–64

UV 327

36.2–38.6

121–129

65–87

UV 571

40.0–44.3

133–148

49–57

UV 360

6.01–7.34

20.0–24.5

35–63

FPSE-UHPLC-MS/MS

Polyester

PDMDPS

60

MeOH

Seawater

UV stabilizers in personal care products

UV P

25

5.63

18.8

-

[20]

UV 329

4.33

14.5

UV 326

8.96

29.9

UV 328

1.63

5.44

UV 327

1.06

3.54

UV 360

2.72

9.08

FPSE-LC-MS/MS

Cellulose

PEG

240

MeOH

River water, Effluent/influent wastewater

Pharmaceuticals Personal care products

MPB

-

10

50

9–27 a

[21]

CBZ

10

50

20–92 a

PrPB

2

20

41–65 a

DHB

5

50

44–74 a

BzPB

1

20

45–67 a

DHMB

2

20

50–74 a

DICLO

1

20

44–73 a

BP-3

2

20

59–93 a

TCC

3

10

57–59 a

TCS

50

200

43–54 a

DFPSE-LC-MS/MS

Cellulose

PEG

10

EtOAc

River water, Effluent/influent wastewater

Pharmaceuticals Personal care products

MPB

-

4

50

12–30 a

[22]

CBZ

4

50

18–53 a

PrPB

2

50

20–64 a

DHB

2

50

21–68 a

BzPB

2

50

33–70 a

DHMB

2

20

39–76 a

DICLO

2

50

23–50 a

BP-3

2

100

45–52 a

TCC

8

50

15–49 a

TCS

20

100

22–43 a

FPSE-GC-MS

Cellulose

PEG

120

EtOAc

River water, Effluent/influent WWTP

Non-steroidal Anti-inflammatory drugs

IBU

418

0.8

3

82–109 b

[23]

NAP

263

2

5

93–111 b

KET

223

5

15

92–108 b

DIC

162

2

7

94–116 b

FPSE-UHPLC-MS/MS

Cellulose

M-PEG

60

MeOH

Wastewater from WWTP, Wastewater from hospital effluent

Cytostatic drugs

ETO

-

7.403

24.68

44.49–78.57

[24]

CP

3.825

12.75

40.50–70.20

VINC

98.04

326.8

42.18–82.82

VINB

39.93

132.8

30.18–101.8

TAM

0.093

0.309

81.90–200.5

Stir-FPSE-UPLC-DAD

Cellulose

PEG

60

MeOH

River-Stream water

Herbicides

Simazine

444

140

460

84–124

[25]

Atrazine

729

240

790

75–126

Secbumeton

988

80

260

76–103

Terbumeton

1165

80

260

75–104

Propazine

996

110

360

75–97

Prometryn

1286

470

1500

78–111

Terbutryn

1411

80

260

78–99

Stir-FPSE-HPLC-DAD

Cellulose

PTHF

15

ACN

Wastewater, Reservoir water

Brominated flame retardants

TBBPA

-

30

-

93

[26]

TBBPA-BAE

20

95

TBBPA-BDBPE

40

92–99

Stir-bar-FPSE-HPLC-DAD

Cellulose

PTHF

10

ACN

Wastewater, Reservoir water

Brominated flame retardants

TBBPA

-

10

-

92–95

[26]

TBBPA-BAE

50

90–97

TBBPA-BDBPE

10

91–98

Food Samples

FPSE-UPLC-MS

Cellulose

PTHF

20

ACN

Food simulants

Non-volatile Additives Migrants

DEP

3.1

5.0 c

15 d

67.6

[8]

TBC

6.4

1.0 c

3 d

104.8

DBM

6.6

3.0 c

10 d

112

TBoAC

7.3

1.0 c

3 d

83.3

TXIB

5.1

1.0 c

3 d

87.4

DBP

5.8

10 c

30 d

91.5

2EHAdip

-

1.0 c

3 d

9.1

2EHseb

2.9

1.0 c

3 d

64.7

IRGA38

-

1.0 c

3 d

78.1

TOPAC

-

5.0 c

15 d

33.3

IRGA1076

12

3.0 c

10 d

80.4

IRGA168

-

3.0 c

10 d

45.7

IRGA1010

-

3.0 c

10 d

67.6

TINU326

11

10 c

25 d

72.1

CHIMA81

1.8

2.0 c

10 d

100.8

TINU327

3.2

10 c

30 d

80.6

CYA1084

-

12 c

30 d

86.5

HAAC12

-

7.0 c

20 d

53.1

FPSE-GC-MS

Cellulose

PEG

60

MeOH

Oranges

Freshness markers

Furfuryl alcohol

-

12.5 c

37.8 d

98.9

[27]

Butyric acid

150 c

445 d

70.1

Cis-3-hexen-1-ol

12.5 c

37.0 d

93.7

Ethyl butyrate

31.1 c

93.4 d

70.5

Vanillin

31.0 c

93.0 d

89.4

Ethyl isovalerate

10.0 c

42.5 d

80.8

Linalool

10.0 c

40.7 d

102.1

1-Octen-3-one

12.5 c

37.6 d

104.1

Eugenol

12.5 c

37.8 d

86.7

Octanal

11.1 c

33.4 d

106.5

Ethyl octanoate

15.0 c

43.6 d

102.6

Limonene

10.0 c

40.8 d

85.4

FPSE-HPLC-DAD

Cellulose

PEG

30

MeOH

Raw milk

Antibiotic drugs Amphenicols

TAP

-

-

-

90.5–103.3

[9]

FFC

92.3–103.3

CAP

97.0–106.0

FPSE-HPLC-UV

Cellulose

PEG

30

MeOH-ACN

Raw milk

Antibiotic drugs Sulfonamides

SMTH

-

-

-

94.7–107.0

[28]

SIX

93.0–104.6

SDMX

96.1–102.5

FPSE-HPLC-DAD

Cellulose

PEG

40

ACN

Intact bovine milk

Antibiotic drugs Penicillin

PENG

-

3.0 c

10.0 d

86.7–115.1

[29]

CLO

6.0 c

20.0 d

82.8–107.2

DICLO

7.5 c

25.0 d

80.8–95.8

OXA

9.0 c

30.0 d

82.6–92.4

FPSE-HPLC-UV

Cellulose

Graphene

40

MeOH-ACN

Cow milk, Human breast milk

Organic monomers

BPA

-

16.7 c

50 d

-

[30]

TEGDMA

UDMA

BisGMA

SAIL-FPSE-HPLC-DAD

Nonwoven Polypropylene

[HMIM]NTf2

2

ACN

Tea

Fungicides

Azoxystrobin

156–161

90–110

300–370

80.3–90.4

[31]

Chlorothalonil

86–93

180–230

600–770

78.1–84.9

Cyprodinil

103

120–170

400–570

79.9–86.4

Trifloxystrobin

217–234

100–120

330–400

81.2–101.2

Biological Samples

FPSE-HPLC-FLD

Cellulose

PHTF

20

MeOH

Urine

Estrogens

BPA

13.9

42

139

90.0–91.0

[12]

E2

14.4

20

66

90.7–90.9

EE2

14.7

36

119

91.0–91.4

FPSE-UHPLC-MS/MS

Cellulose

PTHF

20

MeOH

Urine

Steroid Hormones: Androgens Progestogens

NORET

-

35.2

-

-

[14]

NOR

132.3

MGA

11.1

PRO

12.8

BOL

37.9

NAN

50.1

TES

8.9

DHEA

110.6

AND

80

ADTD

25.6

FPSE-HPLC-PDA

Cellulose

PEG

30

MeOH

Plasma Urine

Antimicrobial drugs Azoles

Ketoconazol

-

30,000

100,000

-

[32]

Terconazole

Voriconazole

Bifonazole

Clotrimazole

Tioconazole

Econazole

Butoconazole

Miconazole

Posaconazole

Ravuconazole

Anditraconazole

FPSE-HPLC-DAD

Cellulose

PEG

20

MeOH-ACN

Blood serum

Drugs Benzodiazepines

APZ

-

10,000

30,000

91.4–106.0

[33]

BRZ

87.6–97.6

DZP

90.0–104.0

LRZ

86.0–102.4

FPSE-HPLC-PDA

Cellulose

PEG PCAP-PDMS-PCAP

30

MeOH

Whole blood Plasma Urine

Inflammatory

Ciprofloxacin

25.8–29.1

20,000–10,0000

50,000–25,0000

-

[34]

bowel disease

Sulfasalazine

56.7–63.9

drugs

Cortisone

26.9–105.4

LOD, Limit of detection, calculated as S/N = 3; LOQ, Limit of quantitation, calculated as S/N = 10; E.T., Extraction time; E.F., Enrichment factor; R%, Relative recovery %; Ref., Reference; a Rapp(%)—Apparent recovery that includes the extraction recovery and matrix effect; b Relative recoveries from calibrations in ultrapure water; c,d LOD and LOQ in ng/g.

2. Fabric Phase Sorptive Extraction: Features of Merit—Comparison with Other Sample Extraction Techniques

Fabric phase sorptive extraction has eloquently integrated both the exhaustive extraction mechanism and the partitioning equilibrium driven extraction into a single technology platform. As such, FPSE possesses the advantages of both sample preparation techniques. Unlike commercially available extraction and micro-extraction techniques, FPSE does not require any special equipment or set-up. The FPSE membrane can be directly introduced into the sampling container for extraction and back-extraction tube for analyte elution. A battery-powered magnetic stirrer can diffuse the solution using a magnetic stir bar. Therefore, the technique is easily field deployable.
Due to the strong chemical bonding between the fabric substrate and the sol-gel sorbents, FPSE membranes can be exposed to any organic or organo-aqueous solvent including a harsh chemical environment (pH 1–13). This offers a unique opportunity for selecting a suitable solvent compatible with both GC and LC and for analyzing simultaneously using both the technique to obtain complementary and holistic chemical information of the sample. On the other hand, the lack of chemical anchorage between the extraction polymer and the substrate limit the solvent selection in most of the classical extraction and micro-extraction techniques.
Although FPSE membranes have been designed as a single use device (like SPE cartridges and disks) to minimize the memory effect from the previous extractions as well as to reduce the risk of cross contamination, it can be reused as many as 50 times without consuming a high volume of organic solvent in the cleaning process.
FPSE eliminates all sample pretreatment steps including filtration, centrifugation, and protein precipitation. It also eliminates solvent evaporation and sample reconstitution from the sample preparation workflow. These steps are often used in SPE.
The extraction time in FPSE varies widely from 20 min to several hours depending on the complexity of the sample matrix and the presence of competing but unwanted compounds in the sample. However, the extraction time can be substantially reduced if FPSE is carried out in a dynamic extraction mode (like an SPE disk). This advantage is only seen in FPSE among all the contemporary sample preparation techniques.
FPSE utilizes sol-gel coating technology for the sorbent coating on the fabric substrates. Unlike the conventional sorbent coating process (physical adhesion of the polymer on the substrate surface followed by free-radical cross-linking reaction), sol-gel coating is a precisely controllable chemical coating process that ensures high batch-to-batch reproducibility, which is a phenomenon of extreme importance in analytical chemistry.
One major advantage of FPSE over other extraction and micro-extraction techniques is its ability to fine tune the overall polarity and selectivity by judiciously selecting the fabric type (hydrophilic or hydrophobic), organic polymer (nonpolar to highly polar), and the inorganic precursor possessing different organic ligands. Conventional extraction and micro-extraction techniques offer limited selectivity towards the target analytes since the organic polymers (in micro-extraction techniques) or the organic ligands (in exhaustive extraction techniques) are the only source of selectivity.
FPSE offers a wide range of sorbents including polar, somewhat polar, nonpolar, cation exchanger, anion exchanger, and mixed mode sorbents. No other extraction and micro-extraction techniques offer such a broad spectrum of sorbent chemistries. In fact, FPSE is the first sample preparation technique that offers traditional SPE sorbents including C8, C18, cyano, diol, phenyl chemistries, and SPME sorbents including poly(dimethylsiloxane) and poly(ethylene glycol) polymeric materials coated on the fabric substrate. As such, FPSE has not only integrated the extraction mechanism of both exhaustive extraction and partitioning equilibrium-based micro-extraction techniques but also makes available all the important sorbent chemistries in both techniques.
In conclusion, FPSE has not only simplified and boosted eco-friendliness in the sample preparation workflow, it has substantially improved the overall sample preparation process.
As an example, Table 2 presents a comprehensive comparison of the performance of the FPSE technique with other sample extraction techniques that have been applied for determining four non-steroidal anti-inflammatory drugs. The selected publications are referred to the analysis using GC-MS so the techniques and numerical data are more comparable. Taking into account the characteristics about the extraction procedure, FPSE can be really practical and easily applicable because it can handle the larger sample volumes and offers the possibility of satisfactory extraction time. Comparing the analytical performance between the techniques, FPSE shows the lowest LOD and LOQ values, which are the most sensitive. In addition, RSDs are below 18% for FPSE, which presents presenting good precision while SPME can be the most repeatable. Lastly, the trueness values, which are expressed as relative recoveries, are quite satisfactory.
Table 2. Comparison of the FPSE with other extraction techniques regarding the determination of four non-steroidal anti-inflammatory drugs known as ibuprofen, naproxen, ketoprofen, and diclofenac.

Extraction Technique

Instrumentation

Sample Volume (mL)

E.T. (min)

LOD ng/L

LOQ ng/L

RSD%

R%

Ref.

FPSE

GC-MS

30

120

0.8–5

3–15

4–18

82–116

[23]

SBSE

GC-MS

15

240

13–21 a

43–70

3–20

77–107

[35]

SPME

GC-MS

22

40

15–40

4–9

[36]

MEPS

GC-MS

5

6

3–110

11–360

3–13

60–160

[37]

LOD, Limit of detection, calculated as S/N = 3; a LOD calculated as blank ±3 SDblank; LOQ, Limit of quantitation, calculated as S/N = 10.

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