目的:建立气相色谱-质谱联用的检测方法测定硅胶管中六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)、十二甲基环六硅氧烷(D6)、十四甲基环七硅氧烷(D7)、十八甲基环九硅氧烷(D9)6个环硅氧烷在pH 3氯化钾溶液、pH 10磷酸氢二钠溶液、0.9%氯化钠溶液、1%吐温80溶液和50%乙醇5种提取溶剂中的提取量。方法:采用HP-5MS毛细管色谱柱(30.0 m×0.25 mm×0.25 μm),数据采集方式为单离子检测扫描(SIM)模式,通过程序升温,以2,6-二叔丁基-4-乙基苯酚(抗氧剂BHEB)为内标,对直接提取得到的提取溶液进行检测。结果:6个环硅氧烷质量浓度在20~1 000 ng·mL-1范围内线性关系良好,检测限和定量限分别为0.9~1.8 ng·mL-1,2.5~14.3 ng·mL-1。在pH 3氯化钾溶液、pH 10磷酸氢二钠溶液、0.9%氯化钠溶液、1%吐温80溶液和50%乙醇5种提取溶剂中回收率均在82.0%~110.9%,RSD均不大于6.4%。在水基提取溶液中没有检测出D4,其他检测到的环硅氧烷浓度均较低,不超过60 ng·mL-1。在50%乙醇提取溶液中检测到D3、D4、D5、D6、D7、D9这6个环硅氧烷,浓度较大但都不超过450 ng·mL-1。结论:检测方法灵敏度高,专属性好,重复性和稳定性也良好,适用于硅胶管中环硅氧烷含量的测定。
Objective: To establish a GC-MS method for the determination of 6 cyclosiloxanes including hexamethylcyclotrisiloxane(D3), octamethylcyclotetrasiloxane(D4), decamethylcyclopentasiloxane(D5), dodecamethylcyclohexasiloxane(D6), tetradecamethylcycloheptasiloxane(D7) and ctadecamethylcyclononasiloxane(D9) in five different extraction media including pH 3 potassium chloride solution, pH 10 disodium phosphate solution, 0.9% sodium chloride solution, 1% Tween 80 solution and 50% ethanol of silicone tubes. Methods: HP-5MS capillary column (30.0 m×0.25 mm×0.25 μm) was used for chromatographic analysis, and the data was collected in a single ion monitoring(SIM) model.The extraction solution was detected by temperature programmed, and 2,6-di-tert-butyl-4-ethylphenol(antioxidant BHEB) was used as internal standard. Results: The mass concentrations of six cyclosiloxanes had good linearity in the range of 20-1 000 ng·mL-1, and LOD and LOQ were 0.9-1.8 ng·mL-1 and 2.5-14.3 ng·mL-1 respectively. The recoveries in pH 3 potassium chloride solution, pH 10 disodium phosphate solution, 0.9% sodium chloride solution, 1% Tween 80 solution and 50% ethanol were between 82.0%-110.9%, with RSDs not greater than 6.4%. No D4 was detected in water-based extraction solutions, the concentration of other cyclosiloxanes was low, less than 60 ng·mL-1. Six cyclosiloxanes(D3, D4, D5, D6, D7 and D9) were detected in 50% ethanol extraction solution,and the concentrations were high but less than 450 ng·mL-1. Conclusion: The detection method has high sensitivity, good specificity, good repeatability and stability. It is suitable for the determination of cyclosiloxane extractionamounts from silicone tubes.
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