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目的建立RP-HPLC法测定膝关节镜手术后罗哌卡因关节腔给药的血浆浓度。方法以曲马多作为内标;采用Hypersil ODS-C_(18)色谱柱(200 mm×4.6 mm,5μm);流动相为乙腈与0.02 mol·L~(-1) NaH_2PO_4缓冲液(用磷酸调pH 3.7,含0.015%三乙胺)梯度洗脱,流速1.0 mL·min~(-1),紫外检测波长220 nm,血样处理以碱性条件下用乙酸乙酯提取,氮气吹干重溶进样,进样量为20μL。关节镜术后在关节腔中注射罗哌卡因150 mg,于0.25、0.5、0.75、1、1.5、2、4、12、16、24 h取血测定罗哌卡因浓度。结果在选定的色谱条件下,曲马多与罗哌卡因保留时间分别约为6.5、10.6 min,罗哌卡因血浆浓度在0.025～4.0 mg·L~(-1)内线性关系良好(r=0.999 9),最低检测浓度为0.01mg·L~(-1),日内、日间精密度RSD<4%,提取回收率为87.79%～89.20%。样品在室温放置24 h及低温冷冻条件下(-20℃)贮存1个月均稳定。关节腔给药后ρ_(max)为(1.01±0.47)mg·L~(-1),t_(max)为(0.75±0.47)h,t_(1/2)为(9.26±6.23)h。结论该方法灵敏简便,准确,重现性较好,可用于罗哌卡因的血药浓度测定。罗哌卡因关节腔内给药较硬膜外给药缓慢平稳释放入血,产生峰浓度较低,血药浓度持续时间较长,为比较安全的给药方法 。
Objective To establish a RP-HPLC method for the determination of plasma concentration of ropivacaine intra-articularly after knee arthroscopy. Methods Tramadol was used as the internal standard. Hypersil ODS-C 18 column (200 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile and 0.02 mol·L -1 NaH 2 PO 4 buffer pH 3.7, containing 0.015% triethylamine) at a flow rate of 1.0 mL · min -1. The UV detection wavelength was 220 nm. The blood samples were extracted with ethyl acetate under basic conditions and dried under nitrogen. Sample injection volume of 20μL. Ropivacaine 150 mg was injected into the articular cavity after arthroscopy. The blood samples were taken for determination of ropivacaine concentration at 0.25, 0.5, 0.75, 1, 1.5, 2, 4, 12, 16 and 24 hours. Results The retention times of tramadol and ropivacaine were about 6.5 and 10.6 min under the selected chromatographic conditions. The plasma concentrations of ropivacaine ranged from 0.025 to 4.0 mg · L -1 r = 0.999 9). The lowest detection concentration was 0.01 mg · L -1. The RSD of intra-day and inter-day RSD was less than 4%, and the recovery rate was 87.79% -89.20%. Samples were stored at room temperature for 24 h and frozen at low temperature (-20 ℃) for 1 month were stable. The ρ max was (1.01 ± 0.47) mg · L -1, the t max was (0.75 ± 0.47) h, and the t 1/2 was 9.26 ± 6.23 h after intra-articular injection. Conclusion The method is sensitive, simple, accurate and reproducible. It can be used for the determination of blood concentration of ropivacaine. Ropivacaine intraarticular administration of epidural drug delivery more slowly and steadily into the blood, resulting in a lower peak concentration, plasma concentration for a longer duration, for a more secure method of administration.