SN/T 5151-2019Determination of seven benzophenones in sunscreen cosmetics by high performance liquid chromatography (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

Please note that some elements of this document may involve patents. Publication of this document the agency is not responsible for identifying these patents.

This standard is proposed and managed by the General Administration of Customs of the People's Republic of China.

This standard was drafted. China Academy of Inspection and Quarantine.

1 Scope

This standard specifies a method for the determination of seven benzophenones in sunscreen cosmetics by high performance liquid chromatography.

This standard applies to the determination of seven benzophenones in lotion and cream sunscreen cosmetics.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document.

GB/T 6682 Analytical laboratory water specifications and test methods

3 Principle

The sample was extracted by solvent, filtered by a microporous membrane, and then determined by high performance liquid chromatography, quantified by external standard method, and confirmed by liquid chromatography-mass spectrometry.

4 Reagents and materials

Unless otherwise specified, the reagents used are of analytical grade, and the water is first-grade water specified in GB/T 6682.

4.1 Methanol. chromatographically pure.

4.2 Tetrahydrofuran. chromatographically pure.

4.3 Standards. 7 benzophenone standard standards Chinese name, English name, CAS number, molecular formula, structural formula, relative molecular weight See Table A in Appendix A. 1. Purity is not less than 95%.

4.4 Standard stock solutions of 7 benzophenones. Accurately weigh each 10mg of each benzophenone standard substance (4.3), accurate to 0.1mg, Put them in 10mL volumetric flasks, dissolve with methanol (4.1) and make up to the mark, shake well, prepare standard stock solutions with concentrations of 1,000µg/mL, store at 4 ° C, and can be used for three months.

4.5 Mixed standard stock solutions of 7 benzophenones. Accurately transfer each standard stock solution (4.4) 1mL to a 20mL volumetric flask in methanol, dilute to the mark with methanol (4.1). The concentration of benzophenones in the solution was 50 µg/mL. 4.6 Mixed standard working solution. Precisely transfer the mixed standard stock solution (4.5) of 7 benzophenones and dilute with methanol (4.1) it is a series of working solutions with a concentration of 0.5 µg/mL, 1 µg/mL, 2 µg/mL, 5 µg/mL, 10 µg/mL, 20 µg/mL, etc.

5 Instruments and equipment

5.1 High Performance Liquid Chromatography (HPLC) instrument. equipped with UV detector or diode array detector.

5.2 Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) instrument. equipped with an electrospray ion source (ESI).

5.3 Analytical balance. Sensitivity is 0.0001g and 0.0001g.

5.4 Centrifuge. The rotation speed is not less than 10,000 rpm.

5.5 Ultrasonic water bath.

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5.6 Vortex mixer.

5.7 Nitrogen blowing instrument.

5.8 Colorimetric tube with stopper. 25mL.

5.9 Plastic centrifuge tube with stopper. 10mL.

5.10 Microporous membrane. 0.45 µm, organic phase.

6 Measurement steps

7 Results calculation

The result is calculated according to formula (1), with two decimal places (the blank value should be deducted from the calculation result).

In the formula.

C --- the content of the target substance in cosmetics, the unit is milligram per kilogram (mg/kg);

D --- dilution factor (if not diluted, it is 1);

rho --- the concentration of the target substance in the sample solution calculated from the standard working curve, the unit is micrograms per milliliter (µg/mL); --- the final constant volume of the sample solution, the unit is milliliter (mL);

8 Low limit of determination

The lower limit of determination of benzophenone-1 and benzophenone-8 in this method is 0.1mg/g, benzophenone-2, benzophenone-3, benzophenone-6 and benzophenone-10.

The lower limit of determination was 0.2 mg/g, and the lower limit of determination of benzophenone-12 was 0.4 mg/g.

9 Recovery rate

The average recovery of the seven benzophenones was 84.9% to 95.2%; the relative standard deviation was 1.7% to 8.5%.

10 Tolerance

The absolute difference between two independent determination results obtained under repeatable conditions should not exceed 10% of the arithmetic mean.

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Appendix A

(Informative appendix) Information of 7 benzophenones

Table A. 1 Information on 7 benzophenones

Chinese name English name CAS No. Molecular formula Structural formula Relative molecular mass Benzophenone-1 Benzotophone-1 1131-56-6 C13H10O3 214.22 Benzophenone-2 Benzotophone-2 2131-55-5 C13H10O5 246.22 Benzophenone-3 3131-57-7 C14H12O3 222.84 Benzophenone-6 Benzotophene-6 6131-54-4 C15H14O5 274.27 Benzophenone-8 Benzoxone-8 131-53-3 C14H12O4 244.42 Benzophenone-10 Benzenophenone-10 1641-17-4 C15H14O3 242.27 Benzophenone-12 Benzophenone-12 12843-05-6 C21H26O3 326.43 SN/T 5151-2019 Appendix B (Informative appendix) HPLC chromatograms of seven benzophenones 1 --- benzophenone-2;

2 --- benzophenone-1;

3 --- benzophenone-8;

4 --- benzophenone-6;

5 --- benzophenone-3;

6 --- benzophenone-10;

7 --- benzophenone-12.

Figure B. 17 high performance liquid chromatograms of seven benzophenones

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Appendix C

(Informative appendix) HPLC-MS confirmation conditions C. 1 HPLC conditions the HPLC conditions are as follows.

a) Chromatographic column. C18, 3.5µm, 150mm × 2.1mm (inner diameter), or equivalent;

b) Mobile phase. See Table C for gradient elution procedure. 1;

c) Flow rate. 0.3mL/min;

d) Column temperature. 30 ° C;

e) Injection volume. 5 µL.

Table C. 1 mobile phase gradient elution procedure

Time/min methanol /% aqueous solution containing 0.1% formic acid /% 3.0 75 25 7.0 85 15 7.1 100 0 11.0 100 0 11.1 75 25 14.0 75 25 C. 2 Mass spectrometry conditions the mass spectrometry conditions are as follows.

a) Ion source. electrospray ion source, positive ion scanning;

b) Capillary voltage. 3.0kV;

c) Extraction voltage. 1.0V;

d) RF lens voltage. 0.1V;

e) Ion source temperature. 150 ° C;

f) Desolvent gas. nitrogen, flow rate 1000L/h, temperature 500 °C;

g) Cone gas. nitrogen, flow rate 50L/h;

h) collision gas. argon;

i) Detection method. multiple reaction monitoring;

ii) See Table C for qualitative ion pair, quantitative ion pair, cone voltage, and collision gas energy of seven benzophenones. 2.

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Table C. 2 Mass spectrometric analysis parameters such as qualitative ion pair, quantitative ion pair, cone voltage and collision gas energy

Chinese name English name Ionization mode monitoring ion pair (m/z) Quantitative ion pair (M/z) Cone voltage (V) Collision energy (EV) Benzophenone-1 Benisotopene-1 ESI + 215.3/137.5125215.3/105.7 7 215.3/137.5 5 25 Benzophenone-2 Benisotopone-2 ESI + 247.3/137.524.77.3/81.8 244.7/137.5 5 21 Benzophenone-3 ESI + 229.4/105.572.294/151.5 5 229.2/151.5 5 26 Benzophenone-6 Benizophenone-6 ESI + 275.3/151.2572.75.3/95.7 7257.15/151.5 5 18 Benzophenone-8 Benisotopene-8 ESI + 245.3/12.162.45.3.15/151.5 5 245.3/12.16 20 Benzophenone-10 Benzophenone-10 ESI + 243.3/15.1525.43.3/119.7. 244.3.3/151.5.20 20 Benzophenone-12 Benzophenone-12 ESI + 327.3/215.34.2327.13/137.6. 327.3/137.6 6 28 SN/T 5151-2019 Appendix D (Informative appendix) Multiple reaction monitoring chromatograms of seven benzophenones

Figure D. 17 Multiple reaction monitoring chromatograms of seven benzophenones

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Figure D. 1 (continued)

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Figure D. 1 (continued)

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Figure D. 1 (continued)

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