Fluorine in toothpaste

Fast and reliable quality control for toothpaste production

Toothpaste and mouthwash contain many ingredients With Time Domain Nuclear Magnetic Resonance
to enhance the quality and health benefits. Fluorine is (TD-NMR), the fluorine content can be accurately
added in typical amounts of 1000 to 1500 ppm to measured irrespective of the fluorine compound and
prevent cavities by strengthening tooth enamel. the toothpaste matrix.
Active ingredients are often sodium fluoride (NaF),
stannous fluoride (SnF2), or sodium monofluorophos- The simplicity and the speed of the analysis make
phate (Na2PO3F). In addition to fluoride, other ingre- TD-NMR the method of choice for production, product
dients can be included to achieve whitening effects development and quality control.
(peroxide) or abrasiveness (silica).
Features and Benefits
The fluorine amount has to be accurately controlled. Most
„„ cost-effective at-line fluorine content
A minimum level of 1000 ppm is needed to provide ­ etermination
d
the desired benefit of strengthening tooth enamel, but Measurement time < 10 min
„„
exceedingly high fluorine amounts can possibly lead to Widely applicable for different toothpaste formulations
„„
health risks (dental fluorosis). Automation option
„„

TD-NMR
Innovation with Integrity
 Application Method Calibration Procedure
The TD-NMR analysis is based on the quantitative and Calibration
„„ range: 250 – 4000 ppm fluorine content
linear signal response from the fluorine nuclei in the Linear
„„ correlation with r² > 0.995
sample. Therefore the amplitude of the NMR signal Coefficient of variance (CV) < 3% for repeated measu-
„„
S (Hahn-Echo) is directly proportional to the soluble rements of a 1000 ppm sample
fluorine mass.

Measurement Calibration Curve

NMR Signal (%/g)

Amplitude

r² = 0.998
/2 3

0
S 0 500 1000 1500 2000 2500 3000 3500 4000

Time Fluorine Concentration (ppm)

Note: Only soluble fluorine is detected due to the very The method is calibrated with 3 to 5 samples of known
fast signal decay of immobilized or insoluble fluorine, fluorine content. Aqueous NaF solutions are recom-
for example in calcium fluoride (CaF2) or magnesium mended as calibration samples. Alternatively, solutions
fluoride (MgF2). The soluble fluorine contributes to the of other APIs may be used. The weight-normalized
desired health benefit. NMR signals (amplitudes) are correlated with the fluo-
rine content by linear regression.
Workflow
Recommended Equipment
Fill sample tube 5 min
mq20
„„ Toothpaste Analyzer
m+
„„ software (21 CFR part 11 compliant)
Solubilize fluorine IQ / OQ Documentation
„„
5 min
by dilution* 26 mm sample tubes
„„
Precision Balance
„„

Temper sample tube Option: Automatic sample changer

„„
30 min
at 40°C**

Run measurement < 10 min

total time
Results (report)
15 -60 min
*optional, depending on formulation ** optional
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Bruker BioSpin

cmr@bruker-biospin.com
www.bruker.com