超声萃取-超高效液相色谱-串联质谱法测定玩具涂层中2种光引发剂残留量  

Determination of Two Photoinitiator Residues in Toy Coatings by Ultrasonic Extraction-UHPLC-MS/MS

作　　者：陶小美 罗小芳 胡爱生 TAO Xiaomei;LUO Xiaofang;HU Aisheng(Eqo Testing and Certification Co.,Ltd.,Kunshan 215331,China;Goodbaby Children's Products Co.,Ltd.,Kunshan 215331,China)

机构地区：[1]亿科检测认证有限公司,昆山215331 [2]好孩子儿童用品有限公司,昆山215331

出　　处：《理化检验（化学分册）》2021年第9期776-780,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省中小企业公共技术服务示范平台建设项目(2020-2023)。

摘　　要：建立了超声萃取-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定玩具涂层中2-二甲氨基-2-苄基-1-[4-(4-吗啉基)苯基]-1-丁酮(光引发剂IHT-PI 910)和2-甲基-1-[4-(甲基硫代)苯基]-2-(4-吗啉基)-1-丙酮(光引发剂IHT-PI 907)残留量的方法。用10 mL乙腈在60℃下超声提取样品30 min,加入0.1%(体积分数,下同)甲酸溶液,过0.20μm滤膜,滤液供UHPLC-MS/MS分析。以ACQUITY UPLC BEH C18色谱柱为固定相,不同体积比的乙腈和0.1%甲酸溶液组成的混合溶液为流动相进行梯度洗脱,目标物经色谱分离后,在电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式下进行质谱分析。结果显示:在优化的试验条件下,2种光引发剂可在3.00 min内完成测定;标准曲线的线性范围均为0.5~100μg·L^(-1),检出限(3S/N)均为1.0μg·L^(-1);对阴性样品进行3个浓度水平的加标回收试验,所得回收率为87.9%~93.4%,测定值的相对标准偏差(n=7)为1.2%~8.6%。用此方法分析了20个随机样品,3个样品检测结果均为阳性,样品2中光引发剂IHT-PI 907的最高检出量为1 528 mg·kg^(-1),超出了REACH法规的限量(1 000 mg·kg^(-1))要求。A method for the determination of 2-benzyl-2-(dimethylamino)-4′-morpholinobutyrophenone(IHT-PI 910) and 2-methyl-4′-(methylthio)-2-morpholinopropiophenone(IHT-PI 907) in toy coatings by ultrasonic extraction-ultra high performance liquid chromatography mass spectrometry(UHPLC-MS/MS) was established. The sample was extracted with 10 mL acetonitrile at 60 ℃ for 30 min, then mixed with 0.1%(volume fraction, the same below) formic acid solution and filtered through 0.20 μm membrane. The filtrate obtained was analyzed by UHPLC-MS/MS. ACQUITY UPLC BEH C18 chromatographic column was used as stationary phase, and mixed solution composed of acetonitrile and 0.1% formic acid solution with various volume ratios was used as mobile phase for gradient elution. The targets separated were analyzed with electrospray ion source positive ion(ESI+) mode and multiple reaction monitoring(MRM) mode. The results showed that under the optimized test conditions, the two photoinitiators could be determined within 3.00 min;linear ranges of the standard curves of 2 targets found were both 0.5-100 μg·L^(-1), with detection limits(3 S/N) of 1.0 μg·L^(-1);the spiked recovery was made on the negative samples at 3 concentration levels, giving values of recovery ranged from 87.9% to 93.4%, and RSDs(n=7) of determined values were in the range of 1.2%-8.6%. This method was used in the analysis of 20 samples, and photoinitiators were detected in 3 samples, with the maximum detection amount of 1 528 mg·kg^(-1) for IHT-PI 907 in No.2 sample, exceeding the limit(1 000 mg·kg^(-1)) specified by REACH regulation.

关 键 词：超声萃取 超高效液相色谱-串联质谱法 2-二甲氨基-2-苄基-1-[4-(4-吗啉基)苯基]-1-丁酮 2-甲基-1-[4-(甲基硫代)苯基]-2-(4-吗啉基)-1-丙酮 光引发剂 玩具涂层 

分 类 号：O657.63[理学—分析化学]