基于安全监管的玄麦甘桔制剂中麦冬投料真实性的考察

Investigation on the authenticity of Ophiopogon japonicus feeding in Xuanmai Ganju preparation based on safety supervision

目的建立玄麦甘桔制剂中山麦冬的掺伪检测方法,考察样品中麦冬的投料状况。方法应用超液相色谱-串联电喷雾三重四级杆质谱技术,采用Ultimate LP-C18色谱柱(100 mm×2.1 mm,1.8μm),以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.2 mL·min-1,柱温为30℃,进样量3μL,采用电喷雾离子源(ESI^(+)),多反应监测(MRM)模式。结果山麦冬(湖北麦冬)的特征成分山麦冬皂苷的线性范围为0.0247~6.185μg·mL^(-1)(r=0.9985),加样回收率为92.50%,RSD为1.88%。同时,以掺伪山麦冬(湖北麦冬)10%作为依据,拟定了检出限度,结果237批次样品中有25批检出山麦冬皂苷B,均为含糖型颗粒剂,检出率为10.5%。结论所用方法准确可靠,可作为玄麦甘桔制剂中山麦冬掺伪的检测方法。

OBJECTIVE To establish a method to detect the adulteration of Liriopes Radix in Xuanmai Ganju preparation,and to investigate the feeding condition of Ophiopogon japonicas(L.f)Ker-Gawl.in samples.METHODS An ultra-high performance liquid chromatography series triple quadrupole mass spectrometry technology was applied.An Ultimate LP-C_(18)column(100 mm×2.1 mm,1.8μm)was adopted,and the acetonitrile-0.1% formic acid solution was used as mobile phase with gradient elution.The flow rate was 0.2 mL·min^(-1),the column temperature was 30℃,and the injection volume was 3μL.Electric spray ion source(ESI^(+))and multiple reaction monitoring(MRM)mode were used.RESULTS The sample injection of liriopesides B had a good linear relationship in the range of 0.0247-6.185μg·mL^(-1)(r=0.9985),and the recovery rate was 92.5%with the RSD of 1.88%.Meanwhile,the detection limit was determined based on 10% of adulterated Liriope spicata(Thunb.)Lour.var.prolifera Y.T.Ma.Among 237 batches of samples,liriopesides B in 25 batches of samples.All of which were sugar-containing granules,with a detection rate of 10.5%.CONCLUSION This method is accurate and reliable,and can be used as the detection method for liriopesides B in Xuanmai Ganju preparation.