液相色谱-串联质谱法测定含植物提取物化妆品中20种农药残留

Determination of 20 Pesticide Residues in Cosmetic Containing Plant Extracts by Liquid Chromatography Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法测定含植物提取物化妆品中20种农药残留,将不同剂型的化妆品基质经乙腈提取、凝胶渗透色谱法净化、浓缩定容,高效液相色谱分离,串联质谱定性和定量检测。结果表明,精吡氟禾草灵在0.5~10μg/L,多菌灵、久效磷和扑灭津在2.5~50μg/L,甲萘威、特乐酚、氟环唑、丁苯吗啉、碘苯腈、禾草敌、西玛津和十三吗啉在5~100μg/L,丁变敌、敌草隆、异恶唑草酮、亚胺菌和利谷隆在25~500μg/L,丙炔氟草胺、异菌脲和炔螨特在50~1000μg/L浓度范围内的线性关系良好,相关系数均大于0.990。20种农药的定量限(LOQ)在0.001~0.1 mg/kg之间,高、中、低3个浓度水平的加标平均回收率为81.5%~116.2%,相对标准偏差(RSD)为0.52%~9.42%。该方法简便、快速、可靠性高,适用于含植物提取物化妆品中农药的检测。

Plants have a long history as the main source and basic raw material of cosmetics.The efficacy and application of plant extracts in cosmetics are becoming more and more extensive.However,environmental pollution causes pesticide residue problems in plant extracts inevitably."Cosmetics Safety Technical Specification(2015 Edition)"stipulates that a variety of pesticide ingredients are prohibited components of cosmetics.Moreover,the first cosmetics regulation EC 1223/2009 also clearly points out that pesticides such as aldrin and dieldrin are prohibited components in cosmetics.In this study,the 20 pesticide components selected as the main research content are all prohibited components specified in the"Cosmetics Safety Technical Specification(2015 Edition)".They have the high detection rate of daily detection and the same detection method.However,due to the lack of testing standards for pesticides in cosmetics at home and abroad,it is difficult to evaluate the pesticides in cosmetics on the domestic market.In particular,for cosmetics containing plant extracts that may contain pesticide residues,there is an urgent need to establish a simple,rapid,efficient and accurate pesticide residue detection and analysis method.Therefore,in order to improve the detection recovery rate,remove the interference of impurity components,reduce the mass spectrometry matrix effect and improve the detection sensitivity,gel permeation chromatography(GPC)purification methods were introduced into the sample pretreatment technology.A sensitive method for determination of 20 banned pesticides residues in cosmetics containing plant extracts by liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established.The target compounds were extracted with acetonitrile followed by GPC for cleanup step and concentrated to a constant volume,separated by high performance liquid chromatography,and then detected by electrospray tandem mass spectrometry qualitatively and quantitatively.The results showed that each target has good linearity in its own content ranges and the correlation coefficients are higher than 0.990.The limit of quantification(LOQ)of 20 pesticides is between 0.001-0.1 mg/kg,the average recovery at three spiked levels is 81.5%-116.2%,and the relative standard deviation(RSD)is 0.52%-9.42%.This method is simple,rapid and reliable,which can be used for determination of 20 pesticides in cosmetics containing plant extracts.This research can not only fill in the domestic and foreign gaps in the standard testing methods for pesticide residues in cosmetics,but also help actively respond to EU-related technical trade measures and guide companies to strengthen their own product quality management.It can provide technical support to improve the domestic and foreign cosmetics standard system,realize the monitoring of pesticide residues in cosmetics and ensure the quality and safety of cosmetics.