| 罗云云,杨欢,陆静娴,郑成,陈碧莲,戴忠.保心宁片(胶囊)中枳壳伪品香圆检查方法的研究[J].中国药事,2023,(1):66-75 |
| 保心宁片(胶囊)中枳壳伪品香圆检查方法的研究 |
| Research on the Detection Method of the Counterfeit Citrus wilsonii for Citrus aurantium in Baoxinning Tablets and Capsules |
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| DOI：10.16153/j.1002-7777.2023.01.008 |
| 中文关键词: 保心宁片(胶囊) 枳壳 香圆 水合氧化前胡素 超高效液相色谱-串联三重四极杆质谱 掺伪 |
| 英文关键词: Baoxinning tablet and capsule Citrus aurantium Citrus wilsonii oxypeucedanin hydrate ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry adulteration |
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| 中文摘要: |
| 目的：建立保心宁片(胶囊)中枳壳伪品香圆的检查方法，为打击中药掺伪提供技术支撑。方法：采用超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF-MS)，Agilent SB C18(100 mm×2.1 mm，1.8 μm)色谱柱，以乙腈和1%甲酸梯度洗脱，流速0.4 mL·min-1，柱温30 ℃；电喷雾离子化(ESI)正离子模式进行检测。采用多元分析统计软件筛选查找枳壳常见伪品香圆的特征性成分水合氧化前胡素，并应用超高效液相色谱-串联三重四极杆质谱(UPLC-QQQ-MS)建立保心宁片(胶囊)中香圆的检查方法。结果：水合氧化前胡素在0.17~1.02 ng范围内线性良好，回归方程： Y=24451X+529.43，r=0.999，精密度RSD为1.8%，稳定性RSD为2.1%，回收率范围为81.1%~86.9%，检测限为0.028 mg·kg-1，定量限为0.092 mg·kg-1。6批样品中有5批检出水合氧化前胡素，1批未检出。 保心宁片(胶囊)中枳壳的处方量为每片(粒)0.5010 g，按照掺伪率10%和转移率30%拟定限度为每片 (粒)2.5μg，4号和5号样品存在掺伪风险。结论：所建方法可用于检查保心宁片(胶囊)中是否存在香圆掺伪情况。 |
| 英文摘要: |
| Objective: To establish the detection method for the adulteration of Citrus aurantium Citrus wilsonii in Baoxinning tablets and capsules to provide technical support for combating the adulteration of traditional Chinese medicine. Methods: The ultra-high performance liquid chromatography-quadrupole timeof-flight mass spectrometry (UPLC-Q-TOF-MS) was used on an Agilent SB C18 (100 mm×2.1 mm, 1.8 µm) column, eluted with a gradient of acetonitrile and 1% formic acid, at a flow rate of 0.4 mL·min-1, the column temperature was 30 ℃, and detected by electrospray ionization (ESI) in positive mode. Multivariate analysis statistical software was used to screen and find for the oxypeucedanin hydrate, a characteristic component of Citrus wilsonii, a common adulterant of Citrus wilsonii. An ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ-MS) method was established to detect whether there is Citrus wilsonii adulteration in Baoxinning tablets and capsules. Results: The concentration of Oxypeucedanin hydratehad good linearity in the range of 0.17-1.02 ng. The regression equation was Y=24451X+529.43, r=0.999, the precision RSD was 1.8%, and the stability RSD was 2.1%, the recovery ranged from 81.1% to 86.9%, the detection limit was 0.028 mg·kg-1, and the quantification limit was 0.092 mg·kg-1. Among the 6 batches of samples, oxypeucedanin hydrate in 5 batches was detected and 1 batch was not detected. The prescription amount of Citrus aurantium in Baoxinning tablets and capsules is 0.5010 g/ tablet (grain), the proposed limit is 2.5 µg/tablet (grain) according to the adulteration rate of 10% and the transfer rate of 30%. There is a risk of adulteration in No. 4 and No. 5 samples. Conclusion: The established method could be used to check whether there is Citrus wilsonii adulteration in Baoxinning tablets and capsules. |
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