Ito Rie, Miura Naoko, Iguchi Hirofumi, Nakamura Hiroko, Ushiro Masaru, Wakui Nobuyuki, Nakahashi Keisuke, Iwasaki Yusuke, Saito Koichi, Suzuki Tsutomu, Nakazawa Hiroyuki
Department of Analytical Chemistry, Hoshi University, 2-4-41 Ebara, Tokyo 142-8501, Japan.
Int J Pharm. 2008 Aug 6;360(1-2):91-5. doi: 10.1016/j.ijpharm.2008.04.020. Epub 2008 Apr 20.
Tris(2-ethylhexyl)trimellitate (TOTM) is used as an alternative plasticizer of polyvinyl chloride (PVC) medical devices. A method for the determination of TOTM released from PVC medical devices into intravenous preparations was developed, which uses liquid chromatography-tandem mass spectrometry (LC-MS/MS). A PVC tube was filled with an intravenous preparation and extraction was carried out by shaking for 1h at room temperature. LC was performed with an Inertsil-C8 (50 mm x 2.1 mm, 5 microm) column. The isocratic mobile phase was acetonitrile:purified water (90:10, v/v) at a flow rate of 0.2 ml/min. MS detection was accomplished with an MS/MS detector equipped with a turbo ionspray ionization source in the positive ion mode. The limit of detection and the limit of quantification for the standard solution of TOTM was 0.5 ng/ml (S/N=3) and 1.0 ng/ml (S/N > or =10), respectively. When Prograf (tacrolimus) was used, the average recovery of TOTM was 101.1% (R.S.D.=4.72%; n=3). When our method was applied to the determination of TOTM released from unsterilized and gamma-ray-sterilized PVC tubes, we found that a higher concentration of TOTM was released from the unsterilized PVC tube than from the gamma-ray-sterilized one.
偏苯三酸三（2-乙基己）酯（TOTM）用作聚氯乙烯（PVC）医疗器械的替代增塑剂。开发了一种测定PVC医疗器械中释放到静脉制剂中TOTM的方法，该方法采用液相色谱-串联质谱法（LC-MS/MS）。将PVC管填充静脉制剂，在室温下振荡萃取1小时。使用Inertsil-C8（50 mm×2.1 mm，5微米）色谱柱进行液相色谱分析。等度流动相为乙腈：纯净水（90:10，v/v），流速为0.2 ml/min。采用配备涡轮离子喷雾电离源的MS/MS检测器在正离子模式下完成质谱检测。TOTM标准溶液的检测限和定量限分别为0.5 ng/ml（S/N = 3）和1.0 ng/ml（S/N≥10）。当使用普乐可复（他克莫司）时，TOTM的平均回收率为101.1%（相对标准偏差=4.72%；n = 3）。当将我们的方法应用于测定未灭菌和γ射线灭菌的PVC管中释放的TOTM时，我们发现未灭菌的PVC管释放的TOTM浓度高于γ射线灭菌的PVC管。
