建立了同时测定尿液中复方α-酮酸片5种有效成分(消旋羟蛋氨酸钙(HMACa)、酮缬氨酸钙(KVCa)、消旋酮异亮氨酸钙(KILCa)、酮亮氨酸钙(KLCa)和酮苯丙氨酸钙(KPACa))的离子对反相高效液相色谱法.分别考察了离子对试剂浓度、缓冲盐浓度和流动相pH值等参数对分离情况的影响.最终采用Waters SymmetryC 18色谱柱(250 mm×4.6 mm,5μm);以乙腈和含15 mmol/L四丁基氢氧化铵的20 mmol/L磷酸盐缓冲液(pH 7.0)为流动相进行梯度洗脱,流速为1.0 mL/min;柱温为35℃;检测波长为210 nm.在上述条件下,5种有效成分得到很好的分离,并且不受尿液中内源性基质的干扰,在20 ～ 200 mg/L范围内线性关系良好(r≥0.999 0);HMACa、KV-Ca、KILCa、KLCa和KPACa的检出限(S/N=3)分别为3.0、5.0、3.6、5.7和2.5 mg/L;定量限(S/N=10)分别为9.6、16.7、12.0、19.0和8.3 mg/L;日间、日内精密度均小于7％;平均回收率在86.79％ ～ 112.00％之间,RSD小于9％(n=5).该方法准确,灵敏度高,重现性好,适用于尿液中这5种有效成分的检测.
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