UPLC/Orbitrap HRMS法测定纺织品中异噻唑啉酮

Rapid determination of isothiazolinones in textiles by UPLC/Orbitrap HRMS

建立了一个快速测定纺织品中5种异噻唑啉酮类抗菌剂的超高效液相色谱，静电场轨道阱高分辨质谱（UPLC／Orbitrap HRMS）方法。该方法以甲醇为萃取溶剂，超声萃取纺织品中的异噻唑啉酮类抗菌剂，提取液经浓缩定容后，进行UPLC／Orbitrap HRMS分析。5种异噻唑啉酮类抗菌剂的色谱分离在Hypersil GOLD色谱柱完成，采用梯度洗脱方式，流动相为0．1％甲酸水溶液／甲醇。质谱分析采用电喷雾正离子模式，5种异噻唑啉酮类抗菌剂的质量准确度误差均小于2×10-6（2mg／kg）。根据提取离子色谱图峰面积采用外标法进行定量。在一定质量浓度范围内，5种异噻唑啉酮类抗菌剂的提取离子色谱峰面积均与其质量浓度线性相关，线性相关系数均大于0．998。在3个不同的添加浓度水平下，平均加标回收率为8113％-92．6％，相对标准偏差为4．0％～9．8％。该方法定性可靠，定量准确，检出限低至0．1μg／kg，可完全满足纺织品中异噻唑啉酮类抗菌剂检测工作的需要。

An effective method is established for the rapid determination of five isothiazolinone antibacterial agents in textiles using ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry （UPLC/Orbitrap HRMS） technique. Isothiazolinone antibacterial agents in textiles are ultrasonically extracted using methanol as an extraction solvent. The extract is concentrated and then detected by UPLC/Orbitrap HRMS. The chromatographic separation of five isothiazolinones is carried out on an Hypersil GOLD column with a gradient elution of methanol and 0.1% aqueous formic acid solution. Five isothiazolinones are detected by orbitrap HRMS in ESI positive mode. Full-scan experiment is carried out. Five isothiazolinones are routinely detected with mass accuracy below 2×10 -6 under the optimal conditions. The quantitative analysis is carried out by the peak area in extracted chromatograms and the external standard method is used in the quantitative analysis. Good linearity is achieved in the respective linear range for five isothiazolinone bacterial agents, with correlation coefficients above 0.998. The blank samples are spiked at three different spiked levels and the spiked average recovery varies from 81.3% to 92.6% while the relative standard deviation （RSD） varies from 4.0% to 9.8%. The limits of detections （LODs） are all 0.1 μg/kg for five isothiazolinones. The proposed method is reliable, accurate and sensitive, and can completely satisfy the demand on the determination of five isothiazolinones in textiles.