尿样中米酵菌酸高效液相色谱法测定

任琳; 秦忠雪; 胡彬; 邹晓莉; 徐先顺; 雍莉

doi:10.11847/zgggws1121040

尿样中米酵菌酸高效液相色谱法测定

Determination of bongkrekic acid in urine with high performance liquid chromatography

摘要

摘要:
目的建立高效液相色谱法测定尿样中米酵菌酸（BA）的含量。
方法尿样经12 000 r/min低温高速离心10 min后，取上层清液直接进样，经C18色谱柱分离，以甲醇 – 乙酸水（pH 2.5）为流动相，等度洗脱，二极管阵列检测器进行检测，以空白基质加标标准曲线进行定量。
结果在0.5～20.0 μg/mL范围内BA具有良好线性关系，相关系数r > 0.998，以3倍信噪比计算，BA的方法检出限为0.3 μg/mL，定量限为1.0 μg/mL，在0.5、1.0、2.0 μg/mL 3 个水平下，加标回收率为87.5 %～113.4 %，相对标准偏差（RSD）为5.5 %～8.4 %。
结论本方法操作简便快捷，准确度好，适用于尿样中BA的测定。

Abstract:
Objective To establish a method for the determination of bongkrekic acid in urine samples.
Methods The urine sample was centrifuged with 12 000 r/min at low temperature for 10 minutes; then the supernatant was directly injected into high performence liqiud chromatography for determination. After separated on a C18 column using methanol and acetic acid water (pH 2.5) as a mobile phase, bongkrekic acid was detected with diode array detector and quantified with blank matrix standard curve.
Results The linear range for bongkrekic acid detection was 0.5 – 20.0 μg/mL; the correlation coefficients were all above 0.998. The detection limit of the method was 0.3 g/mL and the quantitive limit of the method was 1.0 μg/mL. The recovery ranged from 87.5% to 113.4%, with a relative standard deviation (RSD) of less than 8.4%.
Conclusion The established method is simple, rapid, accurate and suitable for the determination of bongkrekic acid in urine sample.

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