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Development and validation of static HS- GC-MS method for simultaneous determination of BTEX in cosmetics : Application of the ISO 12787 for diverse cosmetic formulations

화장품 내 유해물질 BTEX의 HS-GC-MS 동시 분석법 개발 및 유효성 평가: ISO 12787 표준 시험법을 통한 타 화장품 제형으로의 적용

  • 김용준 (KIM YONGJUNE, 아주대학교 일반대학원)

초록/요약

Benzene, toluene, ethylbenzene, and xylene, known as BTEX, are prohibited ingredients in cosmetics due to their toxicity and carcinogenic effects. This study presents the establishment of HS-GC-MS method for determining BTEX in some cosmetic products and its application to other cosmetic formulations following the ISO 12787 approach. For efficient extraction of BTEX and their isotope internal standards (IS) from cosmetic matrices, headspace conditions were developed for salt modifiers, extraction temperature, and time. As the study of optimization, the developed method used a VF-624ms column after headspace extraction at 80°C for 20 min. Mass spectrometry conditions were electron impact (EI) whose temperature of source at 200 °C and quadrupole at 150 °C. Selective ion monitoring was used for subsequent analysis of BTEX and IS. Method validation following the ICH Q2(R1) guideline was carried out for the cosmetic matrices of lotion and cream, essence and oil, toner, and mask. Method validation results showed acceptable performance characteristics including specificity, linearity (R2 ≥ 0.999), detection limit=1.1–3.9 ng/g, quantitation limit=3.2–23.3 ng/g, accuracy=79.9–107.9%, and precision=0.2– 4.5%. The established method was successfully applied to four matrices of cosmetics circulated in Korea. Following the ISO 12787 approach, the developed method was applied to other formulations (cleansers, wet tissues, deodorants, makeup bases, and balms). BTEX were not found in most of the samples and all the parameters were successfully proved, with (recovery 101.1±9.7%, and matrix effect 93.2±8.1%). It is notable that our method can be used to identify the unintentional contamination of BTEX in cosmetic products and contribute to quality control. Keywords Cosmetics; BTEX; HS-GC-MS; Validation; Monitoring; ISO 12787; Simultaneous analysis

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목차

1. Introduction 1
1.1. BTEX as the trace chemical residues in cosmetics 1
1.2. Headspace sampling for analysis of volatile chemicals 2
1.3. ISO 12787 in the cosmetic analysis 5
1.4. The objective of this study 6
2. Materials and methods 7
2.1. Chemicals and reagents 7
2.2. Cosmetic samples 7
2.3. Instrument and apparatus 8
2.4. Analytical method development: Optimization of HS condition 8
2.4.1. Effect of DMSO/water ratio on HS extraction of BTEX 8
2.4.2. Effect of salts on HS extraction of BTEX 9
2.4.3. Effect of CaCl2 concentration on HS extraction of BTEX 9
2.4.4. Optimization of HS equilibrium time 9
2.5. Preparation of STD and IS solution 10
2.6. Preparation of calibrators and samples 10
2.7. HS-GC-MS analytical conditions 10
2.8. Full validation study 13
2.8.1. Specificity 13
2.8.2. Range, linearity, LOD, and LOQ 13
2.8.3. Accuracy and precision 14
2.9. ISO 12787 standard analysis 14
2.9.1. Step 1: Validation criteria using standard solutions 15
2.9.2. Step 2: Sample screening 15
2.9.3. Step 3: Assay 15
3. Results and Discussion 17
3.1. Design of analytical method 17
3.2. Chromatographic separation and SIM ions 19
3.3. Optimization of HS condition 21
3.3.1. Effect of DMSO/water ratio on HS extraction of BTEX 21
3.3.2. Effect of salts on HS extraction of BTEX 23
3.3.3. Effect of CaCl2 concentration on HS extraction of BTEX 25
3.3.4. Optimization of headspace equilibrium time condition 27
3.4. Method validation 29
3.4.1. Specificity 29
3.4.2. Linearity, LOD and LOQ 31
3.4.3. Accuracy and precision 33
3.5. Application to cosmetic samples of LC, EO, T, and M 37
3.6. Application to other cosmetic formulations using ISO 12787 39
3.6.1. Step 1: Minimum validation criteria on standard solutions 39
3.6.2. Step 2: Sample screening 42
3.6.3. Step 3: Assays 42
4. Conclusion 47
Reference 48
5. 국문 초록 52

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