摘要
目的:建立高效液相色谱法测定明目蒺藜丸中绿原酸和木犀草苷含量的方法。方法:采用SHISEIDO CAPCELL PAK C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相以乙腈(A)-0.1%磷酸溶液(B)进行梯度洗脱,流速:1.0 mL·min^(-1),柱温:25℃,检测波长为348 nm。结果:绿原酸和木犀草苷的线性范围分别为0.011 43~0.034 29 mg·mL^(-1)(r=0.999 7)和0.008 716~0.026 15 mg·mL^(-1)(r=0.999 5)。平均回收率分别为99.3%(RSD=1.1%n=9)和98.8%(RSD=1.0%n=9)。4批样品测定结果:绿原酸含量分别为0.17mg·g^(-1)(RSD=0.9%)、0.17 mg·g^(-1)(RSD=1.2%)、0.16 mg·g^(-1)(RSD=0.8%)、0.15 mg·g^(-1)(RSD=1.0%);木犀草苷含量分别为0.15 mg·g^(-1)(RSD=1.0%)、0.13 mg·g^(-1)(RSD=0.8%)、0.13 mg·g^(-1)(RSD=1.1%)、0.11 mg·g^(-1)(RSD=1.3%)。结论:本方法简便、快速、准确,重现性好,适用于明目蒺藜丸的质量控制。
Objective: To establish an HPLC method for determination of chlorogenic acid and galuteolin in Ming- mu Jili pill. Methods: The test was performed in SHISEIDO CAPCELL PAK C18 column(4. 6 mm×250 mm, 5μm) under the gradient elution condition with acetonitrile as the mobile phase A and 0. 1% phosphoric acid solu- tion as mobile phase B. The flow rate was 1.0 mL·min^-1, the column temperature was 25℃ and the detection wavelength was 348 nm. The injection volume was 10μL. Results: The linear ranges of chlorogenic acid and galuteolin fell into 0.011 43 -0.034 29 mg·mL^-1(r =0.999 7) and 0.008 716 -0.026 15 mgmL^-1(r =0. 999 5) with the average recoveries as 99. 3% ( RSD = 1.1% n = 9) and 98.8% ( RSD = 1.0%, n = 9) respectively. The test results of 4 batches of samples were as: 0. 17 mg·g^-1( RSD = 0. 9% ), 0. 17 mg mg·g^-1(RSD = 1.2%), 0. 16 mg·g^-1 (RSD =0. 8%) and 0. 15 mg·g^-1 (RSD = 1.0%) for chlorogenic acid; 0. 15mg·g^-1(RSD=1.0%), 0.13mg·g^-1(RSD=0.8%), 0.13mg·g^-1(RSD=1.1%) and0.11mg·g^-1(RSD = 1.3% ) for galuteolin. Conclusion: This established method is simple, rapid, and accurate with good reproducibility. It can be applicable to the quality control of Mingmu Jili pill.
作者
赵英奎
ZHAO Yingkui(Dandong inspection for drug control, Dandong 118000, China)
出处
《中国药品标准》
CAS
2018年第3期207-212,共6页
Drug Standards of China