RP-HPLC法测定气滞胃痛颗粒中4种成分的含量

目的：建立同时测定气滞胃痛颗粒中白芍药苷、芍药苷、柚皮苷和甘草酸含量的高效液相色谱法。方法：采用Agilent Zorbax SB-C18柱（250 mm×4.6 mm，5 μm），柱温30 ℃；流动相为水（0.2%醋酸）-乙腈（0.2%醋酸），线性梯度洗脱，流速为1.0 mL·min-1；检测波长为230 nm（0-15 min），284 nm（15-20 min），254 nm（20-35 min）。结果：白芍药苷、芍药苷、柚皮苷、甘草酸浓度分别在15.1-226 μg·mL-1（r=0.9998），25.6-383 μg·mL-1（r=0.9998），27.7-277 μg·mL-1（r=0.9998），9.43-47.2 μg·mL-1（r=0.9998）范围内线性关系良好。低、中、高3个浓度的平均加样回收率分别为97.4%-101%（RSD为0.8%-1.7%），96.8%-99.7%（RSD为1.4%-2.6%），97.3%-100%（RSD为1.9%-2.4%）。结论：本方法简便、准确，重复性好，可以为气滞胃痛颗粒的质量控制提供依据。

HPLC-DAD法同时测定气滞胃痛颗粒中5个成分的含量

目的:建立HPLC法同时测定气滞胃痛颗粒中白芍药苷、芍药苷、甘草苷、柚皮苷和新橙皮苷的含量。方法:采用依利特Hypersil C18色谱柱(4.6 mm×150 mm,5μm),以乙腈(A)-水(B)为流动相梯度洗脱(0～45 min,10%A→28%A),流速1.0mL.min-1,采用DAD检测器在200～400 nm波长处进行检测,柱温30℃。结果:调取不同波长的色谱图分别计算各成分的含量,白芍药苷(230 nm)、芍药苷(230 nm)、甘草苷(237 nm)、柚皮苷(283 nm)和新橙皮苷(283 nm)进样量分别在0.12～6.14μg(r=0.9998),0.40～7.92μg(r=0.9998),0.06～3.18μg(r=1.000),0.20～9.84μg(r=0.9999),0.12～6.14μg(r=0.9999)范围内呈现良好的线性关系。平均回收率(n=6)分别为98.1%,98.3%,98.9%,98.6%,97.1%;RSD分别为0.63%,0.69%,0.96%,1.5%,1.3%。结论:该方法快速简便,结果准确可靠,为气滞胃痛颗粒的全面质量控制提供科学的依据。

Pharmacokinetic and tissue distribution studies of paeoniflorin and albiflorin in rats after oral administration of total glycosides of paeony by HPLC-MS/MS

A simple, sensitive and specific high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）method combined with solid phase extraction has been developed and validated for the simultaneous quantification of paeoniflorinand albiflorin in rats plasma and tissue homogenate after administration of total glycosides of paeony （TGP）. Chromatographicseparation was achieved on a C15 column （150 mmx4.6 mm, 5 pro） with mobile phase consisted of acetonitrile-0.05% formicacid aqueous （20： 80, v/v） at a flow rate of 0.5 mL/min. The analytes were detected with triple-quadrupole mass spectrometer usingturbo ion spray with negative ionization in the multiple reaction-monitoring （MRM） modes. The results of method validationconformed to the requirements for the determination of biological samples. This method was successfully applied to thepharmacokinetics and tissue distribution study of TGP in rats. The results showed that paeonifiorin and albiflorin wereabsorbed and reached peak value quickly, and had the similar pharmacokinetic characteristics. Both of them underwent a rapid andwide distribution in the tissues throughout the whole body, among which stomach was the main distribution tissue. Moreover, theyhad the ability to cross the blood-brain barrier.