LC Technical NoteAnalysis of Anionic Surfactants

LT102

GL Sciences Inc.

This application describes the separation of anionic surfactants and toluene in water.
In the Notification No. 261 from the Ministry of Health, Labour and Welfare, Appendix Table 24, a solid-phase extraction
HPLC method is described for the analysis of anionic surfactants.
The cautionary note for this analysis is the potential for detection of toluene as a contaminant peak.
This is because the nonionic surfactant test and equipment used for toluene pretreatment can be shared, and thepresence of toluene in the atmosphere can cause contamination.
Toluene and anionic surfactants were separated using Inertsil ODS-3, a highly retentive column.
(T.Tamura)

Example: Measurement of standard
Toluene addition
1

1. Sodium Decylbenzenesulfonate (C10)
2. Sodium Undecylbenzenesulfonate (C11)
3. Sodium Dodecylbenzenesulfonate (C12)
4. Toluene
5. Sodium Tridecylbenzenesulfonate (C13)
6. Sodium Tetradecylbenzenesulfonate (C14)(1 mg/L)(1 mg/L)(1 mg/L)(1 mg/L)(1 mg/L)(1 mg/L)

Example of pretreatmentusing solid-phase extraction
InertSep RP-1
(250 mg/6 mL)
Conditioning

4400

2Methanol 5 mL
Ultrapure water 5 mL

3Liquid flow

FLU

56200Sample water 500 mL(flow rate 30 mL/min.)

Dehydration

0Elution
02468Time (min)Without toluene

10Methanol 5 mL

12Concentration
To 2 mL as below
Flow nitrogen, at 40 ˚C.

1Constant volume

400

2Adjust the volume to 2 mL

FLU

3HPLC

5Spike recovery test results (reference value)

0200

602468Time (min)1012CompoundRecovery
Rate , %RSD,%1.Sodiumdecylbenzenesulfonamide
2. Sodium undecylbenzenesulfonate
3. Sodium dodecylbenzenesulphonate
4. Sodium tetradecylbenzenesulfonate
5. Tetradecylbenzenesulphonic acid

102.1
99.7
101.5
98.6
97.0

4.1
5.2
4.9
7.0
6.4

Added concentrations are 20 ng/mL, n = 5* Sodium alkylbenzenesulfonate which has the same number of carbons, also
contains branched components and usually has more than one peak.

25000000

HPLC conditions

20000000: Inertsil ODS-3 (5 μm, 150×4.6 mm I.D.)

Elute: 0.1M NaClO4 in CH3CN/H 2 O = 65/35, v/v (isocratic)

Flow rate: 1.0 mL/min

Column temperature : 40 ˚CDetection: FL Ex 221nm Em 284 nm(GL-7453A FL Detector)

Injection volume: 10 μL

15000000

AreaColumn

C10

R² = 0.9998

C11

R² = 0.9998

C12

R² = 0.9998

C13

R² = 0.9999

C14

R² = 0.9999

10000000

5000000

000.2

0.4

0.6

濃度[mg/L][mg/L]
Concentration

Calibration curve

0.81

GL Sciences LC Technical Note

InertSep mini RP-1 250mg 100 /pk

Cat. No. 5010-27000

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We reserve the right to amend this information or data at any time and without any prior announcement.

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