UPLC-MS/MS法检测化妆品中的绿脓菌素和藤黄绿菌素

doi:10.3969/j.issn.2097-2806.2025.08.014

摘要/Abstract

摘要： 建立了测定化妆品中绿脓菌素和藤黄绿菌素的UPLC-MS/MS分析方法。样品经饱和氯化钠溶液分散后，乙腈超声提取，取上层提取液净化分析。采用Phenomenex Kinetex （2.6 µm，50 mm×3.0 mm）柱分离，以0.1%甲酸水-甲醇为流动相进行梯度洗脱，外标法定量。结果表明，两种化合物可在5 min内实现有效分离，在1~100 µg/L质量浓度范围内呈良好的线性关系，相关系数均大于0.993。绿脓菌素和藤黄绿菌素检出限为0.05 mg/kg，定量限为0.10 mg/kg。在0.10，0.25，0.50 mg/kg加标水平下，水剂、膏霜两种典型空白样品的平均回收率为85.58%~102.96%，相对标准偏差（RSD）为1.54%~3.77%，日内（RSD）为0.51%~3.68%，日间（RSD）为1.95%~4.24%。该方法精密度好，准确度高，适用于各种化妆品中绿脓菌素和藤黄绿菌素的测定。

关键词: 超高效液相色谱-串联质谱, 化妆品, 绿脓菌素, 藤黄绿菌素, 检测

Abstract:

A UPLC-MS/MS method for the determination of pyocyanin and pyoluteorin in cosmetics was established. The samples were dispersed by saturated sodium chloride solution in vortex, then acetonitrile was added for ultrasonic extraction, and the upper organic phase was taken for purification analysis. Phenomenex Kinetex （2.6 µm, 50 mm×3.0 mm） column was used for separation. Gradient elution was performed with formic acid water-methanol as mobile phase. External standard method was used for quantification. The results showed that the two compounds could be effectively separated within 5 min, and showed a good linear relationship in the mass concentration range of 1-100 µg/L, with correlation coefficients greater than 0.993. The limits of detection were 0.05 mg/kg, and the limits of quantitation were 0.10 mg/kg. At 0.10, 0.25 and 0.50 mg/kg，the average recoveries of water agent and cream samples ranged from 85.58% to 102.96% and the relative standard deviations （RSD） were 1.54% to 3.77%. The intra-day RSD ranged from 0.51% to 3.68%，and the inter-day RSD ranged from 1.95% to 4.24%. The method has good precision and high accuracy, which is suitable for the determination of pyoluteorin and pyocyanin in various cosmetics.

Key words: UPLC-MS/MS, cosmetics, pyoluteorin, pyocyanin, detection

中图分类号:

TQ658

王璐, 冉丹, 汪辉, 何邵彤, 皮露露, 邓楠. UPLC-MS/MS法检测化妆品中的绿脓菌素和藤黄绿菌素[J]. 日用化学工业（中英文）, 2025, 55(8): 1066-1071.

Lu Wang, Dan Ran, Hui Wang, Shaotong He, Lulu Pi, Nan Deng. Detection of pyoluteorin and pyocyanin in cosmetics using UPLC-MS/MS method[J]. China Surfactant Detergent & Cosmetics, 2025, 55(8): 1066-1071.

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化合物	扫描方式	离子对（m/z）	去簇电压/V	碰撞电压/V
绿脓菌素	ESI⁺	211.1/168.1^a，211.1/196.1	100	46，37
藤黄绿菌素	ESI^-	269.7/135.0^a，269.7/234.0	-80	-26，-24

提取溶剂	绿脓菌素		藤黄绿菌素
提取溶剂	水剂回收率/%	膏霜回收率/%	水剂回收率/%	膏霜回收率/%
乙腈	65.92~70.27	61.07~68.87	58.42~64.30	58.21~64.56
甲醇	60.27~67.69	53.22~61.50	56.52~63.90	51.38~56.12
乙腈/异丙醇	72.21~79.32	71.56~77.24	70.20~73.44	64.35~71.34
甲醇/异丙醇	70.61~74.26	63.20~68.09	65.27~69.07	72.26~75.06
乙腈/饱和氯化钠	78.65~84.33	80.05~83.91	74.27~80.22	72.80~77.60
甲醇/饱和氯化钠	71.34~78.38	71.75~76.33	74.69~81.49	65.01~71.34

净化方式	绿脓菌素		藤黄绿菌素
净化方式	水剂回收率/%	膏霜回收率/%	水剂回收率/%	膏霜回收率/%
PLS固相萃取柱	92.16~94.83	90.88~96.55	94.49~96.14	85.16~92.79
QuEchERS净化盐1	83.93~88.79	81.43~84.29	83.37~88.39	72.25~79.48
QuEchERS净化盐2	85.77~92.13	78.04~84.01	81.23~82.41	77.26~84.79
正己烷	89.67~93.95	84.94~89.44	90.48~96.86	85.19~87.56

化合物名称	水剂			膏霜
化合物名称	加标水平/（mg/kg）	回收率/%	RSD/%	回收率/%	RSD/%
绿脓菌素	0.10	91.53~96.97	2.26	88.97~93.26	1.99
	0.25	94.62~102.96	3.72	89.50~96.22	3.58
	0.50	91.42~100.58	3.77	93.56~98.78	2.22
藤黄绿菌素	0.10	91.19~97.41	2.40	85.58~93.69	3.52
	0.25	90.77~94.12	1.54	90.02~99.35	3.76
	0.50	90.94~99.26	2.97	87.92~92.36	2.64