高效液相色谱法测定阑尾炎症组织中莫西沙星的浓度

Determination of moxifloxacin concentration in inflammatory appendix tissue by HPLC

目的：建立检测阑尾炎症组织中莫西沙星浓度的高效液相色谱方法。方法：分析柱为Kromasil G8柱，流动相为0.02mol·L^-1磷酸二氢钾溶液-甲醇-乙腈（65：20：15，磷酸调节pH3．0），流速1．0mL·min^-1，检测波长296nm，柱温30℃。阑尾组织匀浆后，以二氯甲烷萃取，挥干，用流动相溶解后进样20μL。结果：莫西沙星组织质量浓度在0．08-10.00mg·L^-1范围内线性关系良好．最低定量限为0．08mg·L^-1，最低检测限0．03mg·L^-1；萃取回收率85．6%～92．4％，方法回收率96．0％～102．5％，日内RSD 2．9％～4．6％，日间RSD 5．2％～9．5％；样品在低温冷冻条件下至少3个月稳定。结论：建立的高效液相色谱法准确可靠．可用于测定莫西沙星在阑尾组织中的浓度及其在阑尾组织中的分布研究。

OBJECTIVE To establish an HPLC method for the determination of moxifloxacin in inflammatory appendix tissue. METHODS The separation was performed on a Kromasil C8 column. The mobile phase was consisted of 0. 02 mol·L^-1 KH2PO4 buffer solution, methanol and acetonitrile （65：20： 15, pH adjusted to 3. 00. The flow rate was 1.0 mL·min^-1 and the detection was 296 nm After the inflammatory appendix tissue was homogenized, moxifloxacin was extracted by methylene chloride and enriched, then 20 μL of redissolved solution was injected to the sampler. RESULTS The calibration curve of moxifloxacin tissue concentration was linear in the range of 0. 08-10.00 mg · L^-1. Limit of quantitation （LOQ） was 0. 08 mg· L^-1 ; Limit of detection （LOD） was 0.03 mg·L ^-1 ; the recovery of extraction was 85.6%- 92.4% and the methodological re covery was 96.0%- 102.5%. RSD for within-day precision and between day precision were 2.9%- 4. 6% and 5.2%-9. 5%, re spectively. The moxifloxacin was stable at least within three months under - 80℃. CONCLUSION The established HPLC method is accurate, sensitive and reliable. It could be used for the determination of moxiflocacin in appendix tissue and the study of its tissue distribution.