GB/T 39999-2021Determination of 15 kinds of prohibited quinolone-type antibiotics in cosmetics including enrofloxacin—Liquid chromatography-tandem mass spectrometry (English PDF)

Foreword

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

Introduction

The tested substances in this standard are prohibited substances stipulated in my country's "Safety Technical Specifications for Cosmetics (2015 Edition)".

Prohibited substances refer to substances that cannot be added to cosmetics as raw materials or components in cosmetics production. "Cosmetics Safety Technical Specification (2015 Edition)'' stipulates. If it is technically unavoidable that prohibited substances are brought into cosmetics as impurities, the limited amount of national regulations shall comply with its regulations.

If the limit is not specified, a safety risk assessment should be carried out to ensure that no harm to human health is allowed under normal, reasonable and foreseeable use conditions.

Health hazards. my country has not yet stipulated the limit values of these substances. The formulation of this standard only provides detection methods for the determination of these substances in cosmetics.

1 Scope

This standard specifies the principles, reagents or methods of liquid chromatography-tandem mass spectrometry for 15 banned quinolone antibiotics in cosmetics.

Materials, equipment, test procedures, annual results, recovery rate and precision, tolerances, etc.

This standard is applicable to enoxacin, maribofloxacin, norfloxacin, ofloxacin, ofloxacin, water, emulsion and non-wax-based cream cosmetics.

Fleroxacin, Pefloxacin, Ciprofloxacin, Lomefloxacin, Danofloxacin, Enrofloxacin, Orbifloxacin, Sarafloxacin, Sparfloxacin, Difloxacin Determination of Star and Moxifloxacin.

This standard does not apply to the determination of quinolone antibiotics in powder cosmetics.

The detection limit of 15 quinolone antibiotics in this standard is 0.15mg/kg, and the limit of quantification is 0.50mg/kg.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 6682 Analytical laboratory water specifications and test methods

3 Principle

The 15 quinolone antibiotics in the sample were extracted with acidified acetonitrile. After centrifugation, the extracts were combined and concentrated, and purified with n-hexane. Chromatography-tandem mass spectrometer determination, external standard method quantification.

4 Reagents or materials

Unless otherwise stated, all reagents used are of analytical grade.

4.1 Water, GB/T 6682, level one.

4.2 Acetonitrile. chromatographically pure.

4.3 Formic acid. chromatographically pure.

4.4 n-hexane. chromatographically pure.

4.5 0.1% formic acid acetonitrile solution. accurately measure 1.0mL formic acid (4.3) into a 1000mL volumetric flask, and dilute to the mark with acetonitrile (4.2).

4.6 0.1% formic acid solution. accurately measure 1.0mL formic acid (4.3) into a 1000mL volumetric flask and dilute to the mark with water.

4.7 Constant volume solution. accurately measure 10mL acetonitrile (4.2) and 90mL 0.1% formic acid solution (4.6), and mix.

4.8 Acetonitrile saturated n-hexane solution. Measure 20mL acetonitrile (4.2), add to 50mL n-hexane (4.4), mix well, let stand, and supernatant Liquid reserve.

4.9 Standard material. the purity is not less than 98%, the Chinese name, English name, CAS number, and score of 15 kinds of quinolone antibiotic standard materials The sub-formula, relative molecular mass and chemical structure formula are shown in Table A.1 in Appendix A.

4.10 Mixed standard working solution. accurately weigh appropriate amount of standard substance (4.9) (accurate to 0.1mg), and prepare the quality with acetonitrile (4.2) A single-label standard stock solution with a concentration of 1000µg/mL (stored at 4°C and protected from light, can be stored for 3 months). Accurately transfer the standard stock of each single standard 0.25mL of the solution was placed in a 50mL volumetric flask, and the volume was fixed with acetonitrile (4.2) to prepare a mixed standard intermediate working solution (each 5µg/mL, now prepared use). Take the corresponding blank sample and process it in accordance with 6.1 to obtain the matrix solution. Accurately pipette an appropriate amount of mixed standard intermediate working solution, and use The matrix solution is gradually diluted into a series of mixed mass concentrations of 5.0 µg/L, 10 µg/L, 20 µg/L, 50 µg/L, 100 µg/L, and 200 µg/L. Meet the standard working solution (now equipped and used now).

4.11 Membrane. PTFE membrane with a pore size of 0.22µm.

5 Equipment

5.1 Liquid chromatography-triple quadrupole mass spectrometer. equipped with an electrospray ion source.

5.2 Analytical balance. Sensitivity is 0.001g and 0.0001g.

5.3 Vortex oscillator.

5.4 Ultrasonic cleaner. working frequency is not less than 40kHz.

5.5 Centrifuge. the maximum speed is not less than 4000r/min.

5.6 Nitrogen blowing instrument.

6 Test procedure