High-throughput Screening of 157 Illegally Added Chemical Drugs in Cosmetic by UPLC-Q/Exactive Orbitrap HRMS

OBJECTIVE To establish a method for the high-throughput screening of 157 illegal chemical drugs in cosmetics by ultra-performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q/Exactive Orbitrap HRMS).

METHODS Different pretreatment were applied according to the properties of the analytes: For components No.1–123, samples were ultrasonically extracted with acetonitrile, followed by derivatization(for cyclopirox olamine), dilution with methanol(for tacrolimus and pimecrolimus), or dilution with 0.4% formic acid solution(for other compounds). Separation was performed on an ACQUITY UPLC BEH C₁₈ column(2.1 mm×100 mm,1.7 μm) with a gradient elution using the following mobile phases, respectively: 0.1% formic acid solution-acetonitrile, 0.1% acetic acid-5 mmol ammonium acetate solution-methanol, and water-acetonitrile. For compounds No.124–157, samples were ultrasonically extracted with 20% acetonitrile solution and purified by n-hexane extraction, followed by separation on an ACQUITY UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm) with the mobile phase consisting of 0.1% formic acid-acetonitrile in gradient elution . The flow rate was 0.3 mL·min^–1, the column temperature was 40 ℃ for compounds No.122–123, and 30 ℃ for other analytes. The injection volume was 2 μL. The retention time, accurate masses of precursor ions, and characteristic fragment ions were obtained in both positive and negative ionization modes using a heated electrospray ionization(HESI) source with full-scan/data-dependent MS²(Full MS/dd-MS²) mode. The TraceFinder software was used to establish a screening database for the 157 illegally added chemical drugs.

RESULTS Using this method, 107 batches of commercially available cosmetics were screened. Terbinafine was detected in one batch of children’s skincare products, and nitrofurazone was identified in one batch of acne treatment products.

CONCLUSION The method has high sensitivity, excellent specificity, high detection efficiency, and low experimental cost. It is suitable for high-throughput screening of illegally added drugs in cosmetics and provides technical support for cosmetic safety regulation.