超高效液相色谱-四极杆飞行时间质谱法筛查植物类防脱发化妆品中203种农药残留

Screening of 203 Pesticide Residues in Hair Loss Prevention Cosmetic Containing Plant Extracts by UHPLC-Q-TOF-MS

采用超高效液相色谱-四极杆飞行时间质谱法(UHPLC-Q-TOF-MS)构建了203种农药的质谱数据库,将该数据库用于植物类防脱发化妆品中农药残留的筛查。203种农药单标准溶液经UHPLC-Q-TOF-MS分析后,将获得的各农药母离子和所有子离子质荷比(m/z)及丰度比等质谱数据和保留时间导入UNIFI软件中,得到203种农药数据库。24批液体类化妆品经甲醇提取,离心后,经0.22μm微孔滤膜过滤。以10 mmol·L^(-1)乙酸铵-乙酸溶液(pH 5.0)为水-甲醇流动相的添加剂,以电喷雾离子源正、负离子模式电离,以全信息串联质谱模式采集样品的质谱数据,至少检测1个母离子和1个子离子。将得到的质谱数据与数据库中各农药的保留时间、母离子和子离子m/z及丰度比进行匹配,当满足保留时间绝对偏差的绝对值在0.2 min内,母离子和子离子m/z相对偏差的绝对值小于5×10^(-6),响应强度大于500时,确证样品中含有该农药。结果显示,24批样品中有1批样品检出嘧菌酯。

A mass spectrometry database of 203 pesticides was established by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry(UHPLC-Q-TOF-MS), which was used for the screening of pesticide residues in hair loss prevention cosmetic containing plant extracts. The single standard solutions of 203 pesticides were analyzed by UHPLC-Q-TOF-MS, and the obtained MS information containing mass-to-charge ratio(m/z) of the precursor and product ions and their abundance ratio, as well as retention time of each pesticide were imported into UNIFI software to establish the database of 203 pesticides. The 24 batches of liquid cosmetics were extracted with methanol. After centrifugation, the solution was filtered by 0.22 μm microporous membrane. The mobile phase containing water and methanol was supplemented 10 mmol·L^(-1)ammonium acetate-acetic acid solution(pH 5.0), and electrospray ionization source with positive and negative modes was used for ionization. MS data of the samples were collected with data-independent acquisition mass spectrometry mode, and at least one precursor ion and one product ion were detected. The MS data obtained were matched with the retention time, m/z and abundance ratios of the precursor and product ions of pesticide in the database. When the absolute value of the absolute deviation of retention time was within 0.2 min, the absolute values of the relative deriations of m/z of precursor and product ions were less 5×10^(-6), and the intensity response was greater than 500, it was indicated that the pesticide was confirmed in the sample. The results showed that azoxystrobin was detected in one from 24 batches of the samples.