Objective: To control the quality of Bovis Calculus in Niuhuang Qingxin pills(prescription of the bureau) by establishing an LC-MS/MS characteristic chromatogram for bile acids. Methods: LC-MS/MS characteristic chromatogram analysis was performed on a Waters SymmetryshieldTM C18(250 mm×4.6 mm, 5μm) with the gradient elution of 0.2% formic acid solution(containing 10 mmol·L-1 of ammonium acetate)(A)-acetonitrile(B) at a flow rate of 1.0 mL·min-1. The electrospray ion (ESI) resource was negative mode and monitoring ion pairs were glycocholic acid(m/z 464.3→m/z 402.4/74.1), taurocholic acid (m/z 514.3→m/z 124.1/80.0), cholic acid(m/z 407.4→m/z 343.3/289.1), hyodeoxycholic acid(m/z 391.4→m/z 391.4), chenodeoxycholic acid(m/z 391.4→m/z 391.4) and deoxycholic acid(m/z 391.4→m/z 343.3/327.2). Results: The LC-MS/MS characteristic chromatogram of bile acids in Bovis Calculus was established in Niuhuang Qingxin pills (prescription of the bureau). The specific value of peaks area of bile acids in Bovis Calculus and its substitutes were different.Bovis Calculus and its substitutes could be identified according to the specific value of peak area of taurocholic acid to cholic acid and whether hyodeoxycholic acid was detected. There was an adulteration use of Bovis Calculus Artifactus in Niuhuang Qingxin pills (prescription of the bureau). The types of Bovis Calculus and its substitutes in other batches were consistent with those in the instructions. Conclusion: LC-MS/MS characteristic chromatogram technology can effectively eliminate the interference of other ingredients in Niuhuang Qingxin pills(prescription of the bureau). The established characteristic chromatogram of bile acids can be used to identify the types of Bovis Calculus and its substitutes in Niuhuang Qingxin pills (prescription of the bureau), which provides reference for the quality control of Bovis Calculus in Niuhuang Qingxin pills (prescription of the bureau).
HU Xiao-ru, NIE Li-xing, HE Feng-yan, LIU Jing-jing, DAI Zhong, MA Shuang-cheng
. Identification of Bovis Calculus and its substitutes in Niuhuang Qingxin pills (prescription of the bureau) by LC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(10)
: 1808
-1814
.
DOI: 10.16155/j.0254-1793.2022.10.14
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