超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法同时检测补中益气丸中毛蕊异黄酮葡萄糖苷、橙皮苷、甘草酸铵的含量

doi:10.3976/j.issn.1002-4026.2023.02.003

Abstract

Abstract:

In this study, we have developed a novel method for the simultaneous determination of calycosin 7-O-glucoside, hesperidin, and ammonium glycyrrhizinate in Buzhongyiqi Pills based on UPLC-Q/Orbitrap HRMS using Hypersil Gold C₁₈ chromatographic column. The gradient mobile phase comprised acetonile as well as water containing 0.1% formic acid. The flow rate, column temperature, and injection volume were 0.4 mL/min, 40 ℃, and 1 μL, respectively. Mass spectrometer was operated using an electrospray ionization source in the positive ion mode for detection. The scan range was 100~1 500 m/z. Quantification was performed by extracting the accurate mass of the target compounds.The linear ranges of calycosin 7-O-glucoside,hesperidin, ammonium glycyrrhizinate were 0.089 1~1.425 0 μg/mL,0.098 4~12.600 0 μg/mL, and 7.425 0~29.700 0 μg/mL (r≥0.999 3), respectively. Furthermore, the limits of detection were 5.57 ng/mL, 4.10 ng/mL, and 5.80 ng/mL, respectively, while the limits of quantitation were 22.26 ng/mL, 12.30 ng/mL, and 23.20 ng/mL, respectively. The results demonstrated good precision, repeatability, and sample stability. Spike recoveries were 91%~105%(δ_RSD≤5.0%,n=6). This method is simple, accurate, and highly sensitive, which is suitable for the simultaneous determination of calycosin 7-O-glucoside, hesperidin, and ammonium glycyrrhizinate in Buzhongyiqi Pills.

Key words: UPLC-Q/Orbitrap HRMS, Buzhongyiqi Pills, calycosin 7-O-glucoside, hesperidin, ammonium glycyrrhizinate

CLC Number:

R284.1

WU Dan, HUANG Biyun, WANG Jing, LIU Long. Simultaneous determination of calycosin 7-O-glucoside, hesperidin, and ammonium glycyrrhizinate in Buzhongyiqi Pills via UPLC-Q/Orbitrap HRMS[J].Shandong Science, 2023, 36(2): 16-22.

Figures/Tables 6

Table 1

Fig.1

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Table 2

Table 3

Table 4

References 16

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名称	分子式	保留时间/min	理论质量数	实际定量质量数	质量偏差
毛蕊异黄酮葡萄糖苷	C₂₂H₂₂O₁₀	5.75	447.128 6[M+H⁺]	447.128 2	0.9×10^-6
橙皮苷	C₂₈H₃₄O₁₅	6.34	611.197 0[M+H⁺]	611.196 8	0.3×10^-6
甘草酸铵	C₄₂H₆₅NO₁₆	8.08	823.411 1[M-NH₃+H⁺]	823.410 6	0.6×10^-6

待测成分	回归方程	相关系数r	线性范围/(μg·mL^-1)
毛蕊异黄酮葡萄糖苷	Y=5.83×10⁶X+2.98×10⁶	0.999 6	0.09~1.43
橙皮苷	Y=1.81×10⁷X+2.57×10⁶	0.999 3	0.09~12.60
甘草酸铵	Y=3.46×10⁶X+2.46×10⁷	0.999 4	7.43~29.70

待测成分	称样量/g	样品中含量/μg	加入量/μg	检出量/μg	回收率/%	平均回收率/%	δ_RSD/%
	0.504	41.11	32.4	67.88	92.34
毛蕊异黄酮葡萄糖苷	0.501	40.87	41.3	75.28	91.61	96.32	4.61
	0.510	41.60	49.2	87.51	96.38
	0.504	78.48	62.0	128.10	91.19
橙皮苷	0.501	78.02	78.5	165.02	105.43	94.95	4.73
	0.510	79.42	93.8	162.23	93.66
	0.504	1 486.94	1 192.0	2 801.10	104.56
甘草酸铵	0.501	1 478.09	1 490.0	2 741.32	92.36	95.56	4.91
	0.510	1 504.64	1 785.0	3 358.03	102.08

批号	毛蕊异黄酮葡萄糖苷	橙皮苷	甘草酸铵	厂家
202201194	81.57	155.72	2 950.27	九芝堂股份有限公司
211004	51.20	1 050.96	2 991.62	仲景宛西制药股份有限公司
20220123	44.35	152.32	2 953.11	江西药都樟树制药有限公司

Simultaneous determination of calycosin 7-O-glucoside, hesperidin, and ammonium glycyrrhizinate in Buzhongyiqi Pills via UPLC-Q/Orbitrap HRMS

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