UPLC-MS/MS检查川贝清肺糖浆中掺加的川贝母伪品

Adulteration Situation of Frritillaira in Chuanbei Qingfei Syrup by UPLC-MS/MS

关键词:  川贝清肺糖浆  川贝母伪品  生物碱  超高效液相色谱-质谱联用

Key words:  Chuanbei Qingfei syrup  counterfeit Frritillaira  alkaloids  UPLC-MS/MS

摘要:

目的 建立超高效液相色谱-串联电喷雾三重四级杆质谱(UPLC-MS/MS)法检查川贝清肺糖浆中掺加的川贝母伪品。方法 样品经碱化稀释，采用BEH C₁₈(2.1 mm×100 mm，1.7 μm)色谱柱；流动相为乙腈-5 mmol·L^-1乙酸铵(含0.1%甲酸)，梯度洗脱；电喷雾离子源(ESI⁺)，多反应检测(MRM)模式检测正品川贝母和其混淆品种的自制对照糖浆以及50批川贝清肺糖浆中5种生物碱(贝母辛、西贝母碱、西贝母碱苷、贝母素甲、贝母素乙)。结果 能否检出西贝母碱和西贝母碱苷可以区分正品川贝母与湖北贝母、浙贝母和平贝母在川贝清肺糖浆中的投料情况，50批川贝清肺糖浆中有5批未检出西贝母碱和西贝母碱苷，疑似使用川贝母伪品投料。结论 该方法操作简单，灵敏度高，结果稳定可靠，可用于筛查川贝清肺糖浆中川贝母伪品投料的情况。

Abstract:

OBJECTIVE To establish the detection method for the determination of counterfeit Frritillaira in Chuanbei Qingfei syrup by UPLC-MS/MS. METHODS The samples were diluted, and separated on a BEH C₁₈(2.1 mm×100 mm, 1.7 μm) column.The mobile phase were acetonitrile and 5 mmol×L^‒1 ammonium acetate(containing 0.1% formic acid) with gradient elution. The 5 alkaloids in genuine Fritillaria chuanensis and its confounded varieties of homemade control syrup and 50 batches of Chuanbei Qingfei syrup were detected by electrospray ion source(ESI⁺) and multiple reaction detection(MRM) mode. The 5 alkaloids were sipeimine-3β-D-glucoside, peimine, peiminine, sipeimine, peimsine. RESULTS The detection of sifritiline and sifritiline glycosides could distinguish the feeding conditions of genuine Fritillaria chuanensis, Hubei Fritillaria chuanensis, Zhejiang Fritillaria chuanensis and Fritillaria chuanensis in the Chuanbei Qingfei syrup. In the 50 batches of Chuanbei Qingfei syrup, sifritiline and sifritiline glycosides were not detected in 5 batches, which was suspected of using counterfeit Fritillaria chuanensis. CONCLUSION This method has the advantages of high selectivity, high sensitivity and simple sample extraction, and can be used to screen counterfeit Frritillaira in Chuanbei Qingfei syrup.