化妆品样品前处理与检测技术研究进展

doi:10.3724/SP.J.1123.2019.06031

色谱 ›› 2020, Vol. 38 ›› Issue (2): 151-161.DOI: 10.3724/SP.J.1123.2019.06031

• 特别策划：第22届全国色谱学术报告会优秀论文专栏 • 上一篇下一篇

化妆品样品前处理与检测技术研究进展

郭项雨¹, 陈萌¹^,², 孟宪双¹, 吕悦广¹^,³, 张楠¹^,⁴, 连显会¹^,⁴, 王春¹^,⁵, 高海燕¹^,⁶, 马强¹^,^*()

¹ 中国检验检疫科学研究院, 北京 100176
² 北京中医药大学中药学院, 北京 102488
³ 中国科学院大学化学科学学院, 北京 100049
⁴ 大连理工大学生命与医药学院, 辽宁盘锦 124221
⁵ 南京农业大学资源与环境科学学院, 江苏南京 210095
⁶ 内蒙古自治区产品质量检验研究院, 内蒙古呼和浩特 010070

收稿日期:2019-07-15 出版日期:2020-02-08 发布日期:2020-12-10
通讯作者: 马强
作者简介:马强.Tel:(010)53897463, E-mail:maqiang@caiq.org.cn
基金资助:
中央级公益性科研院所基本科研业务费专项资金资助项目(2019JK008)

Research progress in sample pretreatment and analytical techniques for cosmetics

GUO Xiangyu¹, CHEN Meng¹^,², MENG Xianshuang¹, Lü Yueguang¹^,³, ZHANG Nan¹^,⁴, LIAN Xianhui¹^,⁴, WANG Chun¹^,⁵, GAO Haiyan¹^,⁶, MA Qiang¹^,^*()

¹ Chinese Academy of Inspection and Quarantine, Beijing 100176, China
² School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 102488, China
³ School of Chemical Science, University of Chinese Academy of Sciences, Beijing 100049, China
⁴ School of Life Science and Medicine, Dalian University of Technology, Panjin 124221, China
⁵ College of Resources and Environmental Sciences, Nanjing Agricultural University, Nanjing 210095, China
⁶ The Inner Mongolia Autonomous Region Institute of Product Quality Inspection, Huhhot 010070, China

Received:2019-07-15 Online:2020-02-08 Published:2020-12-10
Contact: MA Qiang
Supported by:
Basic Research Fund for Central Public Interest Institutes(2019JK008)

摘要/Abstract

摘要：

随着我国经济和人民生活水平的不断提高，作为日常消费品的化妆品产业发展迅猛，其安全性日益受到广泛关注。随之而来的化妆品检测量的大幅增长对检测技术提出了更高的要求。传统样品前处理和检测技术因有机试剂消耗量大，检测通量低、检测周期长已无法满足当前绿色化学发展和高通量检测的需求。对此，科研人员开发了一系列环境友好型前处理技术以及高通量现场快速检测方法，为化妆品质量安全保驾护航。该文综述了当前化妆品样品前处理及检测技术的研究进展，并展望了其发展趋势和应用前景，以期为从事化妆品检测的科研和检验人员提供技术参考。

关键词: 样品前处理, 检测技术, 化妆品, 综述

Abstract:

With the continuous economic development and improvement of living standards, cosmetic products are being widely used as daily consumer products, and there are increasing concerns about their safety. Consequently, there is a substantial increase in the number of cosmetic samples subjected to various analyses, and this in turn necessitates more stringent requirements for the related analytical techniques. However, traditional sample pretreatment and analytical techniques are time-consuming, require large amounts of organic solvents, and have low throughput, thus failing to meet the current demand for green analytical chemistry. To address this issue, researchers have developed numerous environmentally friendly pretreatment techniques as well as high-throughput and rapid on-site methods to ensure the quality and safety of cosmetics. This paper reviews the current progress in sample pretreatment and analytical techniques for cosmetics and discusses the trends and prospects, which may provide technical guidance for researchers and inspectors in the analysis of cosmetic products.

Key words: sample pretreatment, analytical techniques, cosmetics, review

郭项雨, 陈萌, 孟宪双, 吕悦广, 张楠, 连显会, 王春, 高海燕, 马强. 化妆品样品前处理与检测技术研究进展[J]. 色谱, 2020, 38(2): 151-161.

GUO Xiangyu, CHEN Meng, MENG Xianshuang, Lü Yueguang, ZHANG Nan, LIAN Xianhui, WANG Chun, GAO Haiyan, MA Qiang. Research progress in sample pretreatment and analytical techniques for cosmetics[J]. Chinese Journal of Chromatography, 2020, 38(2): 151-161.

图/表 6

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Category	Compounds	Recoveries/%	RSDs/%	Reference
Preservative	13 preservatives, such as 5-bromo-5-nitro-1, 3-dioxane, bronopol, methyl-p-hydroxybenzoate, and tert-butyl-p-hydroxy anisole	88-110	＜10	[12]
Plasticizer and synthetic musk	18 plasticizers, such as dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, and dibutyl phthalate; 12 synthetic musk, such as traseolide, musk xylene, tonalide, and musk moskene	85-105	＜8	[13]
Spice allergen	25 spice allergens, such as limonene, benzyl alcohol, linalool, methyl 2-octynic acid ester, and citronellol	＞75	＜10	[14]
Preservative	methyl isothiazolinone, methyl chloroisothiazolinone, benzoisothiazolinone, and octyl isothiazolinone	＞80	＜7	[15]
Spice allergen, preservative, plasticizer and musk	26 spice allergens, such as α-pinene, limonene, benzyl alcohol, linalool, and methyl 2-octynic acid ester; 13 preservatives, such as 5-bromo-5-nitro-1, 3-dioxane, phenoxyethanol, and methyl p-hydroxybenzoate; 15 plasticizers, such as dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, and dibutyl phthalate; 12 musks, such as musk ambrette, traseolide, galaxolide, and musk xylene	80-110	＜15	[16]
Spice allergen and preservative	25 spice allergens, such as limonene, benzyl alcohol, linalool, and methyl 2-octynic acid ester; 13 preservatives, such as phenoxyethanol, methyl p-hydroxybenzoate, butylated hydroxyanisole, and dibutyl hydroxytoluene	＞90	＜10	[17]
Dyestuff	9 dyestuffs, such as ponceaux SX, acid orange 7, sunset yellow FCF, and allura red AC	70-120	＜15	[18]
Preservative	11 preservatives, such as methyl benzoate, ethyl benzoate, butyl benzoate, phenyl benzoate, and triclosan	＞92 (methyl benzoate 50, ethyl benzoate 70)	＜8	[19]
Dyestuff	19 dyestuffs, such as acid yellow 36, ponceaux SX, acid red 14, and acid orange 7	69.5-121	1.1-15	[20]
Colorant	63 colorants, such as acid blue 1, acid blue 7, acid green 3, and acid green 9	64-128.4	0.9-10.1	[21]

Category	Compounds	Recoveries/%	RSDs/%	Reference
Preservative	13 preservatives, such as 5-bromo-5-nitro-1, 3-dioxane, bronopol, methyl-p-hydroxybenzoate, and tert-butyl-p-hydroxy anisole	88-110	＜10	[12]
Plasticizer and synthetic musk	18 plasticizers, such as dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, and dibutyl phthalate; 12 synthetic musk, such as traseolide, musk xylene, tonalide, and musk moskene	85-105	＜8	[13]
Spice allergen	25 spice allergens, such as limonene, benzyl alcohol, linalool, methyl 2-octynic acid ester, and citronellol	＞75	＜10	[14]
Preservative	methyl isothiazolinone, methyl chloroisothiazolinone, benzoisothiazolinone, and octyl isothiazolinone	＞80	＜7	[15]
Spice allergen, preservative, plasticizer and musk	26 spice allergens, such as α-pinene, limonene, benzyl alcohol, linalool, and methyl 2-octynic acid ester; 13 preservatives, such as 5-bromo-5-nitro-1, 3-dioxane, phenoxyethanol, and methyl p-hydroxybenzoate; 15 plasticizers, such as dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, and dibutyl phthalate; 12 musks, such as musk ambrette, traseolide, galaxolide, and musk xylene	80-110	＜15	[16]
Spice allergen and preservative	25 spice allergens, such as limonene, benzyl alcohol, linalool, and methyl 2-octynic acid ester; 13 preservatives, such as phenoxyethanol, methyl p-hydroxybenzoate, butylated hydroxyanisole, and dibutyl hydroxytoluene	＞90	＜10	[17]
Dyestuff	9 dyestuffs, such as ponceaux SX, acid orange 7, sunset yellow FCF, and allura red AC	70-120	＜15	[18]
Preservative	11 preservatives, such as methyl benzoate, ethyl benzoate, butyl benzoate, phenyl benzoate, and triclosan	＞92 (methyl benzoate 50, ethyl benzoate 70)	＜8	[19]
Dyestuff	19 dyestuffs, such as acid yellow 36, ponceaux SX, acid red 14, and acid orange 7	69.5-121	1.1-15	[20]
Colorant	63 colorants, such as acid blue 1, acid blue 7, acid green 3, and acid green 9	64-128.4	0.9-10.1	[21]

Category	Compounds	Extraction solvent	Dispersing solvent	Recoveries/%	RSDs/%	Reference
[C₆MIM][PF₆]: 1-hexyl-3-methylimidazolium hexafluorophosphate; ACN-Tr-114: acetonitrile-Triton X-114; -: not mentioned.
Preservative	methylparaben, ethylparaben, propylparaben, butylparaben, sorbic acid, benzoic acid, and salicylic acid	trichloromethane	isopropyl alcohol	71.1-112.6	-	[38]
Paraben	methylparaben, ethylparaben, propylparaben, butylparaben, isobutylparaben, and isoamylparaben	n-octanol	water	93.5-104.3	＜4.8	[39]
Colorant	rhodamine B and rhodamine 6G	1-octanol	acetone	90.3-94.7	＜5	[40]
Colorant	acid yellow 23, acid blue 74, acid red 18, acid yellow 1, sunset yellow FCF, allura red, brilliant blue FCF, basic red 51, orange I, acid red 87, acid red 51, metanil yellow, acid orange 3, and acid violet 43	tetrahydrofuran	ethanol-water (95:5, v/v)	90.2-106.1	0.30-3.1	[41]
Metal ion	mercury	[C₆MIM][PF₆]	methanol	86.7-101.2	-	[42]
Natural compound	atranol and chloroatranol	chloroform	acetone	79-106	9	[43]
Vitamin	vitamin E	carbon tetrachloride	acetonitrile	87-105	＜7.8	[44]
Paraben	methylparaben, ethylparaben, propylparaben, isobutylparaben, butylparaben, and isoamylparaben	chloroform	tetrahydrofuran	81.0-103	＜8.2	[45]
Phthalate ester	benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, di-n-butyl phthalate, diethyl phthalate, dimethyl phthalate, and di-n-octyl phthalate	carbon tetrachloride	acetonitrile	84-124	＜10	[46]
Metal ion	nickel	chloroform	ethanol	97-99	1.2	[47]
Organic solvent	formaldehyde	water	acetonitrile	91-113	＜9.2	[48]
Caine-type prohibited ingredient	tricaine, benzocaine, procaine, risocaine, chloroprocaine, lidocaine, tetracaine, amylocaine, pramocaine, and butacaine	n-dodecyl alcohol	tetrahydrofuran	70.7-94.7	1.2-12.7	[49]
UV filter	benzophenone, 4-hydroxybenzophenone, 2, 4-dihydroxybenzophenone, and 2-hydroxy-4-methoxybenzophenone	[C₆MIM][PF₆]	ACN-Tr-114	80.2-117.7	2.8-10.6	[50]
Pesticide residue	hexachlorophene	[C₆MIM][PF₆]	methanol	74.5-97.7	3.8-6.7	[51]

Category	Compounds	Extraction solvent	Dispersing solvent	Recoveries/%	RSDs/%	Reference
[C₆MIM][PF₆]: 1-hexyl-3-methylimidazolium hexafluorophosphate; ACN-Tr-114: acetonitrile-Triton X-114; -: not mentioned.
Preservative	methylparaben, ethylparaben, propylparaben, butylparaben, sorbic acid, benzoic acid, and salicylic acid	trichloromethane	isopropyl alcohol	71.1-112.6	-	[38]
Paraben	methylparaben, ethylparaben, propylparaben, butylparaben, isobutylparaben, and isoamylparaben	n-octanol	water	93.5-104.3	＜4.8	[39]
Colorant	rhodamine B and rhodamine 6G	1-octanol	acetone	90.3-94.7	＜5	[40]
Colorant	acid yellow 23, acid blue 74, acid red 18, acid yellow 1, sunset yellow FCF, allura red, brilliant blue FCF, basic red 51, orange I, acid red 87, acid red 51, metanil yellow, acid orange 3, and acid violet 43	tetrahydrofuran	ethanol-water (95:5, v/v)	90.2-106.1	0.30-3.1	[41]
Metal ion	mercury	[C₆MIM][PF₆]	methanol	86.7-101.2	-	[42]
Natural compound	atranol and chloroatranol	chloroform	acetone	79-106	9	[43]
Vitamin	vitamin E	carbon tetrachloride	acetonitrile	87-105	＜7.8	[44]
Paraben	methylparaben, ethylparaben, propylparaben, isobutylparaben, butylparaben, and isoamylparaben	chloroform	tetrahydrofuran	81.0-103	＜8.2	[45]
Phthalate ester	benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, di-n-butyl phthalate, diethyl phthalate, dimethyl phthalate, and di-n-octyl phthalate	carbon tetrachloride	acetonitrile	84-124	＜10	[46]
Metal ion	nickel	chloroform	ethanol	97-99	1.2	[47]
Organic solvent	formaldehyde	water	acetonitrile	91-113	＜9.2	[48]
Caine-type prohibited ingredient	tricaine, benzocaine, procaine, risocaine, chloroprocaine, lidocaine, tetracaine, amylocaine, pramocaine, and butacaine	n-dodecyl alcohol	tetrahydrofuran	70.7-94.7	1.2-12.7	[49]
UV filter	benzophenone, 4-hydroxybenzophenone, 2, 4-dihydroxybenzophenone, and 2-hydroxy-4-methoxybenzophenone	[C₆MIM][PF₆]	ACN-Tr-114	80.2-117.7	2.8-10.6	[50]
Pesticide residue	hexachlorophene	[C₆MIM][PF₆]	methanol	74.5-97.7	3.8-6.7	[51]

Category	Compounds	Extraction method	Reference
Preservative	methyl benzoate, ethyl benzoate, butyl benzoate, phenyl benzoate, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, butyl paraben, benzyl 4-hydroxybenzoate, triclosan, 2, 6-di-tert-butyl-4-methylphenol, and butylated hydroxyanisole	direct solid phase microextraction	[19]
Antioxidant and preservative	butylated hydroxyanisole, butylated hydroxytoluene, methylparaben, ethylparaben, iso-propylparaben, and iso-butylparaben	headspace solid phase microextraction	[64]
Biomarker volatile	3-methyl-1-butanol, 2-heptanone, 2-nonanone, 1-undecene, 2-phenylethanol, 1-nonanol, 1-decanol, 2-undecanone, indole, 2-undecanol, undecanal, 1-undecanol, 3-dodecanone, 1-dodecanol, 2-tridecanone, 2-tridecyl alcohol, tridecanal, tridecyl alcohol, myristic aldehyde, tetradecanol, 2-pentadecanone, and 1-pentadecanol	headspace solid phase microextraction	[65]
Organic reagent	methanol	headspace solid phase microextraction	[66]
Organic reagent	carbon tetrachloride	headspace solid phase microextraction	[67]
Organic reagent	formaldehyde	headspace solid phase microextraction	[68]

化妆品样品前处理与检测技术研究进展

Research progress in sample pretreatment and analytical techniques for cosmetics

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Metrics

Category	Compounds	Type of solvent	Solvent	Recoveries/%	RSDs/%	Reference
THF: tetrahydrofuran; -: not mentioned.
Paraben	methyl paraben, ethyl paraben, and propyl paraben	ionic liquid	1-butyl-3-methylimidazolium hexafluorophosphate	55.3-102.8	-	[70]
Paraben	methyl paraben, ethyl paraben, propyl paraben, and butyl paraben	ionic liquid	1-butyl-3-methylimidazolium chloride	80.3-110.2	≤14.9	[76]
Pigment	disperse yellow 3, pigment orange 5, sudan Ⅰ, sudan Ⅱ, sudan Ⅲ, sudan Ⅳ, and sudan blue Ⅱ	ionic liquid	1-octyl-3-methylimidazolium hexafluorophosphate	80.4-106.0	-	[77]
Dye	brilliant blue FCF	ionic liquid	1-decyl-3-methylimidazolium tetrafluoroborate	98.6-102.8	-	[78]
Benzophenone	benzophenone, 4-hydroxybenzophenone, 2, 4-dihydroxybenzophenone, and 2-hydroxy-4-dihydroxybenzophenone	ionic liquid	1-hexyl-3-methylimidazolium hexaflfluorophosphate	80.2-117.7	≤10.6	[79]
Hormone	17α-estradiol, 17α-ethinylestradiol, estrone, 17α-hydroxy-progesterone, medroxyprogesterone, megestrol-17-acetate, norethisterone acetate, and progesterone	ionic liquid	1-hexyl-3-methylimidazolium tetraflfluoroborate	93.2-114.2	≤5.2	[80]
Dyestuff	rhodamine B	deep eutectic solvent	tetrabutyl ammonium chloride-decanoic acid	97-110	-	[72]
Preservative	methyl paraben, ethyl paraben, propyl paraben, and butyl paraben	supramolecular solvent	1-decanol-THF-water	86-102	≤5.2	[74]
Preservative	methyl paraben, ethyl paraben, and propyl paraben	supramolecular solvent	propanol-gemini surfactant C₁₄C₂C₁₄-water	90.3-107.9	≤13.3	[81]
Benzene serie	benzene, toluene, ethylbenzene, p-xylene, m-xylene, and o-xylene	aqueous two-phase system	isopropanol-(NH₄)₂SO₄-H₂O	81.1-98.2	≤4.99	[75]

Category	Compounds	Method	LODs	LOQs	Reference
UPLC-Q-TOF MS: ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry; UPLC-LTQ Orbitrap MS: ultra high performance liquid chromatography coupled with linear ion trap quadrupole Orbitrap mass spectrometry; -: not mentioned.
Coumarin	18 coumarin compounds, such as dihydrocoumarin, 7-hydroxycoumarin, 6-methoxy-7-hydroxycoumarin, and 7-methylcoumarin	UPLC-Q-TOF MS	-	10-60 μg/kg	[86]
Plant efficacy component	4 functional ingredients, such as quercetin, naringin, and rutin	UPLC-Q-TOF MS	-	0.03-0.1 mg/kg	[87]
Glucocorticoid	86 glucocorticoids, such as prednisolone, cortisone, fluorometholone, and dexamethasone	LC-Q-TOF MS	-	0.02-0.05 mg/kg	[88]
Ultraviolet absorber	12 ultraviolet absorbers, such as phenylbenzimidazolesulfonic acid, p-aminobenzoic acid, benzophenone-4, and octocrylene	HPLC-Q-TOF MS	0.001%-0.2%	-	[93]
Brightener	12 brighteners, such as kojic acid, arbutin, hydroquinone, nicotine, and salicylic acid	HPLC-Q-TOF MS	0.099-30.15 μg/L	-	[94]
Colorant	4 colorants, such as malachite green and crystal violet	UHPLC-LTQ Orbitrap MS	≤5 μg/kg	-	[95]
Hormone	24 hormones, such as cortisone, beclomethasone, and fludrocortisone acetate	UPLC-LTQ Orbitrap MS	≤10 μg/kg	-	[96]
Antibiotic	36 sulfadiazines, such as sulfamethoxine, sulfamethoxine, trimethoprim, and sulfamethazine	UHPLC-LTQ Orbitrap MS	≤10 μg/kg	-	[90]
Five categories of antibiotic, hormones, etc.	89 compounds, such as antibiotics (fluoroquinolones, sulfonamides, chloramphenicol, and nitroimidazoles), hormones (glucocorticoids, estrogens, androgens, and progestins), phthalates, pesticide residue, malachite green, and crystal violet	UPLC-LTQ Orbitrap MS	-	5-10 μg/kg	[97]
Glucocorticoid	12 compounds, such as prednisolone, prednisone, methylprednisolone, and flumetasone	UPLC-Q Orbitrap MS	1-2 μg/kg	3-5 μg/kg	[98]
Five categories of antibiotic, glucocorticoid, etc.	100 compounds including 39 antibiotics, 40 glucocorticoids, 9 androgens, 8 progestogens, and 4 antifungal drugs	UHPLC-Q Orbitrap MS	1.1-16 μg/kg	3.6-42.5 μg/kg	[92]
Colorant	63 colorants, such as acid blue 1, acid blue 7, acid green 3, acid green 9, and acid red 50	UHPLC-Q Orbitrap MS	0.0005-0.1 mg/kg	0.002-0.2 mg/kg	[21]
Phthalate	14 phthalate compounds, such as butyl benzyl phthalate, di(2-methoxy)ethyl phthalate, di(2-ethyl)hexyl phthalate, and di(4-methyl-2-pentyl) phthalate	UPLC-LTQ Orbitrap MS	0.05-0.5 mg/kg	-	[91]

Category	Compounds	Ambient ionization	MS	LODs	Reference
PABA: para aminobenzoic acid; ND-EESI: neutral desorption extractive electrospray; DART: direct analysis in real time; LTP: low temperature plasma; LIT: linear ion trap; IMS: ion mobility spectrometry; TOF: time of flight.
Dyestuff	sudan Ⅰ, sudan Ⅱ, sudan Ⅲ, and sudan Ⅳ	paper spray	miniature MS	5-30 μg/kg	[104]
Preservative	propyl p-hydroxybenzoate, isobutyl p-hydroxybenzoate, amyl p-hydroxybenzoate, and phenyl p-hydroxybenzoate	extractive nanoESI	miniature MS	5-25 μg/kg	[104]
Antibiotic	chloramphenicol and metronidazole	extractive nanoESI	miniature MS	20 μg/kg, 10 μg/kg	[104]
Hormone	epistotesterone	slug flow microextraction	miniature MS	5 μg/kg	[104]
Sunscreen	phenyl benzimidazole sulfonic acid, diethylhexyloxyphenol methoxyphenyl triazine, 4-aminobenzoic acid, and oxybenzone	ND-EESI	LIT MS	0.09~10 μg/kg	[114]
Moisturizer	diethylene glycol and ethylene glycol	DART	Orbitrap MS	3-34 μg/g	[115]
Antibiotic	gatifloxacin, enoxacin, pefloxacin, metronidazole, metimidazole, ornidazole, nitrofurantoin, and nitrofurazone	extractive nanoESI	IMS	20 μg/kg	[111]
Preservative	3, 4′, 5-tribromo salicylanilide, 4′, 5-dibromo salicylanilide, and 3′, 4′-dichlorosalicylbenzene	paper spray, extractive nanoESI	IMS	50 μg/kg	[112]
Coumarin	hydrogen coumarin, 7-methylcoumarin, 7-methoxycoumarin, 7-ethoxy-4-methylcoumarin, and dicoumarin	paper spray, extractive nanoESI	IMS	1-2.25 mg/kg	[113]
Anti-inflammatory agent	glycyrrhizic acid, polyethylene glycol monostearate, and tocopheryl acetate	DART	TOF MS	-	[116]
Moisturizer	diethylene glycol	DART	Orbitrap MS	-	[117]
Preservative	methylparaben and butyl p-hydroxybenzoate	DART	TOF MS	0.14-0.3 μg/g	[118]
Sunscreen	benzophenone-3, dimethyl PABA, ethylhexyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, and ethylhexyl salicylate	LTP	LTQ FT ICR MS	0.13-7.67 μg/g	[119]

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