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Article(id=1241322674052460814, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241322661654098823, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202309365, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1695052800000, receivedDateStr=2023-09-19, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773883988153, onlineDateStr=2026-03-19, pubDate=1706112000000, pubDateStr=2024-01-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773883988153, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773883988153, creator=13701087609, updateTime=1773883988153, updator=13701087609, issue=Issue{id=1241322661654098823, tenantId=1146029695717560320, journalId=1227665162245664772, year='2024', volume='51', issue='2', pageStart='193', pageEnd='384', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773883985198, creator=13701087609, updateTime=1773890256678, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241348966214849502, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241322661654098823, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241348966214849503, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241322661654098823, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=322, endPage=327, ext={EN=ArticleExt(id=1241322674966819137, articleId=1241322674052460814, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Qualitative and quantitative determination of 13 triterpenoids in Wolfiporia cocos from Yunnan by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry, columnId=1228016572065837304, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective

To realize rapid qualitative and quantitative detection of 13 triterpenoids in Wolfiporia cocos from Yunnan by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry.

Methods

Triterpenoids in Wolfiporia cocos were extracted by ultrasonic extraction (methanol). The separation was carried on an ACQUITY UPLC © HSS C18 column (2.1 mm×50mm, 1.7μm) with, 10 mmol/L ammonium formate-0.1% formic acid aqueous solution and acetonitrile as mobile phase. The gradient elution flow rate was 0.5ml/min, with the column temperature of 30℃. Negative ion multiple reaction monitoring mode was used for detection. Qualitative and quantitative analysis using secondary mass spectrometry and accurate molecular weight.

Results

13 triterpenoids in Wolfiporia cocos were good with in the linear ranges (r≥0.99). The spiked recoveries were from 80.35% to 116.92%, with relative standard deviations of 1.88% to 9.7%. 13 triterpenoids were detected in Wolfiporia cocos samples, and the total contents were between 79 433-85 900 mg/kg.

Conclusion

The method is simple, accurate, efficient and sensitive, and it is suitable for the qualitative and quantitative detection of 13 triterpenoids in Wolfiporia cocos.

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目的

利用超高效液相色谱-四级杆-飞行时间质谱（UPLC-Q-TOF)快速定性定量检测茯苓中13种茯苓三萜类化合物。

方法

利用超声萃取法（甲醇）对茯苓中三萜类化合物进行提取。采用ACQUITY UPLC © HSS C18柱（2.1 mm×50 mm, 1.7μm）分离,10 mmol/L乙酸铵-0.1%甲酸水溶液(A)和乙腈（B）为流动相梯度洗脱，流速为0.5 ml/min,柱温30℃,采用负离子多反应监测模式进行检测，利用精确分子量和二级质谱定性定量。

结果

13种茯苓三萜类化合物在线性范围内线性关系良好（r2≥0.99），样品加标回收率（n=6）为80.35%～116.92%，相对标准偏差为1.88%～9.7%，在茯苓药材中13种茯苓三萜类化合物均被检测出，检出量在79 433～85 900 mg/kg之间。

结论

此方法操作简便、准确、高效、灵敏，适用于茯苓药材中主要三萜类化合物的定性定量检测。

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林佶，E-mail：
, copyrightStatement=本刊刊出的所有文章不代表中华预防医学会和本刊编委会的观点，除非特别声明。, copyrightOwner=中华预防医学会和四川大学华西公共卫生学院, extLink=null, articleAbsUrl=null, sourceXml=4WpToJlM3329vCmqzkBfeg==, magXml=eIOn2aPaZYOvmWQorMKvXg==, pdfUrl=null, pdf=UC8rAuzuQdejMOm9rKoLoQ==, pdfFileSize=805496, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=o9NycZz7FZrZGoe6k/7Anw==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=E7qaRRU74EvNR68j47k/9A==, mapNumber=null, authorCompany=null, fund=null, authors=

孙明月（1996—），女，硕士在读，研究方向：公共卫生

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孙明月（1996—），女，硕士在读，研究方向：公共卫生

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Research on processing technology and quality of poria cocosin different seasons and weather[J]. Farm Products Processing, 2018, (6): 20-22, 27., articleTitle=Research on processing technology and quality of poria cocosin different seasons and weather, refAbstract=null)], funds=[Fund(id=1241322686236914481, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, awardId=2023Y0944, language=CN, fundingSource=云南省教育厅科学研究基金项目(2023Y0944), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1241322678448091626, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, xref=1., ext=[AuthorCompanyExt(id=1241322678464868845, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, companyId=1241322678448091626, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=School of Public Health, Dali University, Dali, Yunnan 671000, China), AuthorCompanyExt(id=1241322678473257455, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, companyId=1241322678448091626, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.大理大学公共卫生学院，云南 大理 671000)]), AuthorCompany(id=1241322678586503674, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, xref=2., ext=[AuthorCompanyExt(id=1241322678594892284, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, companyId=1241322678586503674, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.昆明医科大学公共卫生学院)]), AuthorCompany(id=1241322678712332805, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, xref=3., ext=[AuthorCompanyExt(id=1241322678720721414, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, companyId=1241322678712332805, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.云南省疾病预防控制中心理化实验室)])], figs=[ArticleFig(id=1241322682675950277, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Fig.1, caption=The chromatogram of standard solution, figureFileSmall=v2eKcJ0f2k9aVNHdeZlW/w==, figureFileBig=o9NycZz7FZrZGoe6k/7Anw==, tableContent=null), ArticleFig(id=1241322682801779406, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=图1, caption=标准溶液色谱图

峰号：1、6α-猪苓酸C；2、16α-羟基松苓新酸；3、去氢土莫酸；4、土莫酸；5、猪苓酸C；6、3-表去氢土莫酸；7、3-O-乙酰基-16α-羟基松苓新酸；8、3-O-乙酰基-16α-羟基去氢松苓新酸；9、去氢茯苓酸；10、茯苓酸；11、松苓新酸；12、栓菌酸；13、齿孔酸。

, figureFileSmall=v2eKcJ0f2k9aVNHdeZlW/w==, figureFileBig=o9NycZz7FZrZGoe6k/7Anw==, tableContent=null), ArticleFig(id=1241322683036660440, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Fig.2, caption=The mass spectrogram of 13 triterpenoids, figureFileSmall=KCVOgXKHrfUhHrpMl5a6Aw==, figureFileBig=qNH9vIEV2VZ0YMQvTLY80w==, tableContent=null), ArticleFig(id=1241322683133129438, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=图2, caption=13种三萜类化合物的质谱图

注：1、6α-猪苓酸C；2、16α-羟基松苓新酸；3、去氢土莫酸；4、土莫酸；5、猪苓酸C；6、3-表去氢土莫酸；7、3-O-乙酰基-16α-羟基松苓新酸；8、3-O-乙酰基-16α-羟基去氢松苓新酸；9、去氢茯苓酸；10、茯苓酸；11、松苓新酸；12、栓菌酸；13、齿孔酸。

, figureFileSmall=KCVOgXKHrfUhHrpMl5a6Aw==, figureFileBig=qNH9vIEV2VZ0YMQvTLY80w==, tableContent=null), ArticleFig(id=1241322683250569955, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Fig.3, caption=The chromatogram of a sample, figureFileSmall=5C81k6J6YEQ+idOuGc3P8A==, figureFileBig=LgueTpPOMmU2LlyxiqMPbQ==, tableContent=null), ArticleFig(id=1241322683355427559, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=图3, caption=某样品色谱图

注：每个峰的编号所指物质与图1相同。

, figureFileSmall=5C81k6J6YEQ+idOuGc3P8A==, figureFileBig=LgueTpPOMmU2LlyxiqMPbQ==, tableContent=null), ArticleFig(id=1241322683477062381, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 1, caption=

The gradient elution procedure

, figureFileSmall=null, figureFileBig=null, tableContent=
时间（min）流动相A（%）流动相B(%)
0.0098.02.00
1.5030.070.0
3.0022.078.0
5.0010.090.0
6.0098.02.00
), ArticleFig(id=1241322683602891507, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表1, caption=

梯度洗脱程序

, figureFileSmall=null, figureFileBig=null, tableContent=
时间（min）流动相A（%）流动相B(%)
0.0098.02.00
1.5030.070.0
3.0022.078.0
5.0010.090.0
6.0098.02.00
), ArticleFig(id=1241322683674194680, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 2, caption=

Ion source parameters

, figureFileSmall=null, figureFileBig=null, tableContent=
项目参数
离子模式ESI-
毛细管电压4.0kV
雾化器温度250 ℃
雾化器压35 psi
干燥气流速13.0 L/min
鞘流气流速12.0 L/min
鞘流气温度350 ℃
参比离子m/z 112.99、m/z 601.98、m/z 1 033.99
扫描范围m/z 50～1 100
), ArticleFig(id=1241322683745497853, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表2, caption=

离子源参数

, figureFileSmall=null, figureFileBig=null, tableContent=
项目参数
离子模式ESI-
毛细管电压4.0kV
雾化器温度250 ℃
雾化器压35 psi
干燥气流速13.0 L/min
鞘流气流速12.0 L/min
鞘流气温度350 ℃
参比离子m/z 112.99、m/z 601.98、m/z 1 033.99
扫描范围m/z 50～1 100
), ArticleFig(id=1241322683841966851, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 3, caption=

Mass spectrometric parameters

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物分子式保留时间
（min）		相对分子质量(Mr)碰撞能量
（V）		碎片离子
（m/z）
6α-羟基猪苓酸CC31H46O51.89498.365497.33a，108.02，171.98
3-表去氢土莫酸C31H48O42.54484.455483.35a，423.31，407.29
去氢土莫酸C31H48O42.21484.458483.85a，421.31，389.28
3-O-乙酰-16α-羟基氢化松苓新酸C32H50O52.98514.760513.36a，251.87，288.29
猪苓酸CC31H46O42.43482.360481.33a，120.04，384.82
齿孔酸C31H50O34.54470.455469.37a，112.99，154.97
松苓新酸C30H46O33.91454.360453.34a，112.99，323.23
栓菌酸C30H48O34.12456.460455.35a，390.71，236.03
茯苓酸C33H52O53.24528.460527.37a，523.20，350.36
3-O-乙酰基-16α-羟基松苓新酸C32H48O52.85512.460511.34a，492.71，480.84
去氢茯苓酸C33H50O53.08526.460525.36a，144.00，505.26
16α-羟基松苓新酸C30H48O42.09470.360469.33a，448.50，461.34
土莫酸C31H50O42.26486.460485.36a，148.60，423.32
), ArticleFig(id=1241322683946824456, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表3, caption=

质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物分子式保留时间
（min）		相对分子质量(Mr)碰撞能量
（V）		碎片离子
（m/z）
6α-羟基猪苓酸CC31H46O51.89498.365497.33a，108.02，171.98
3-表去氢土莫酸C31H48O42.54484.455483.35a，423.31，407.29
去氢土莫酸C31H48O42.21484.458483.85a，421.31，389.28
3-O-乙酰-16α-羟基氢化松苓新酸C32H50O52.98514.760513.36a，251.87，288.29
猪苓酸CC31H46O42.43482.360481.33a，120.04，384.82
齿孔酸C31H50O34.54470.455469.37a，112.99，154.97
松苓新酸C30H46O33.91454.360453.34a，112.99，323.23
栓菌酸C30H48O34.12456.460455.35a，390.71，236.03
茯苓酸C33H52O53.24528.460527.37a，523.20，350.36
3-O-乙酰基-16α-羟基松苓新酸C32H48O52.85512.460511.34a，492.71，480.84
去氢茯苓酸C33H50O53.08526.460525.36a，144.00，505.26
16α-羟基松苓新酸C30H48O42.09470.360469.33a，448.50，461.34
土莫酸C31H50O42.26486.460485.36a，148.60，423.32
), ArticleFig(id=1241322684055876363, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 4, caption=

The gradient elution procedure

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时间（min）流动相A（%）流动相B(%)
0.0098.02.0
1.5030.070.0
3.0022.078.0
5.0010.090.0
6.0098.02.0
), ArticleFig(id=1241322684198482705, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表4, caption=

梯度洗脱程序

, figureFileSmall=null, figureFileBig=null, tableContent=
时间（min）流动相A（%）流动相B(%)
0.0098.02.0
1.5030.070.0
3.0022.078.0
5.0010.090.0
6.0098.02.0
), ArticleFig(id=1241322684324311830, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 5, caption=

The linear regression equations, correlation coefficients, limits of detection, limits of quantitation and stability of the method

, figureFileSmall=null, figureFileBig=null, tableContent=
分析物线性回归方程相关系数
（r）		检出限/（ng/ml）定量限/（ng/ml）稳定性/
（%）
6α-羟基猪苓酸CY=932.43X+736.360.999 74.314.03.19
3-表去氢土莫酸Y=1 366.88X-3 087.940.999 94.716.02.24
去氢土莫酸Y=1 999.77+3 103.200.998 51.96.22.70
3-O-乙酰-16α-羟基氢化松苓新酸Y=452.96X+382.700.999 72.48.12.32
猪苓酸CY=2 978.47X-26 412.250.995 62.37.74.36
齿孔酸Y=3 352.28X-31 863.950.997 53.411.04.36
松苓新酸Y=6 895.30X-61 389.200.998 76.521.53.58
栓菌酸Y=1 997.23X+122.150.999 86.321.05.27
茯苓酸Y=2 573.09X-15 292.580.997 64.013.04.25
3-O-乙酰基-16α-羟基松苓新酸Y=2 176.42X-11 155.930.998 14.515.02.15
去氢茯苓酸Y=2 834.24X-15 416.690.999 53.311.03.87
16α-羟基松苓新酸Y=2 278.15X-6 004.970.998 02.27.04.10
土莫酸Y=1 999.77X+3 103.200.998 52.58.42.95
), ArticleFig(id=1241322684433363741, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表5, caption=

方法的线性回归方程、相关系数、检出限、定量限和稳定性

, figureFileSmall=null, figureFileBig=null, tableContent=
分析物线性回归方程相关系数
（r）		检出限/（ng/ml）定量限/（ng/ml）稳定性/
（%）
6α-羟基猪苓酸CY=932.43X+736.360.999 74.314.03.19
3-表去氢土莫酸Y=1 366.88X-3 087.940.999 94.716.02.24
去氢土莫酸Y=1 999.77+3 103.200.998 51.96.22.70
3-O-乙酰-16α-羟基氢化松苓新酸Y=452.96X+382.700.999 72.48.12.32
猪苓酸CY=2 978.47X-26 412.250.995 62.37.74.36
齿孔酸Y=3 352.28X-31 863.950.997 53.411.04.36
松苓新酸Y=6 895.30X-61 389.200.998 76.521.53.58
栓菌酸Y=1 997.23X+122.150.999 86.321.05.27
茯苓酸Y=2 573.09X-15 292.580.997 64.013.04.25
3-O-乙酰基-16α-羟基松苓新酸Y=2 176.42X-11 155.930.998 14.515.02.15
去氢茯苓酸Y=2 834.24X-15 416.690.999 53.311.03.87
16α-羟基松苓新酸Y=2 278.15X-6 004.970.998 02.27.04.10
土莫酸Y=1 999.77X+3 103.200.998 52.58.42.95
), ArticleFig(id=1241322684546609954, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=EN, label=Table 6, caption=

Recoveries and prelative standard deviation of the method（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
分析物加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）		加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）		加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）
6α-羟基猪苓酸C20105.4±10.29.70200104.8±4.74.53500101.1±2.32.43
3-表去氢土莫酸20103.2±9.49.11200105.1±3.33.31500109.5±2.11.88
去氢土莫酸2095.58±8.68.97200112.2±4.43.91500113.2±3.83.38
3-O-乙酰-16α-羟基氢化松苓新酸20107.0±7.817.30200115.3±5.14.43500110.7±8.37.45
猪苓酸C2097.92±5.75.82200106.8±4.64.29500103.9±4.74.53
齿孔酸2090.67±5.25.75200103.4±3.83.65500107.5±3.22.97
松苓新酸2097.08±9.39.54200103.8±4.74.50500104.0±2.12.02
栓菌酸2080.75±3.574.4320091.58±3.94.2950092.67±2.42.61
茯苓酸2099.08±7.77.77200103.9±3.73.5850099.63±2.32.30
3-O-乙酰基-16α-羟基松苓新酸20100.92±5.85.74200100.9±6.66.5250080.35±39.38.76
去氢茯苓酸2098.42±5.96.00200107.3±6.56.0650081.97±39.672.01
16α-羟基松苓新酸2097.83±8.68.83200107.58±3.83.53500111.47±3.12.74
土莫酸2092.58±7.98.53200116.92±3.12.68500106.4±3.23.00
), ArticleFig(id=1241322684672439081, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241322674052460814, language=CN, label=表6, caption=

方法的加标回收率和相对标准偏差（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
分析物加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）		加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）		加标浓度
(ng/ml)		回收率±标准差（%）RSD
（%）
6α-羟基猪苓酸C20105.4±10.29.70200104.8±4.74.53500101.1±2.32.43
3-表去氢土莫酸20103.2±9.49.11200105.1±3.33.31500109.5±2.11.88
去氢土莫酸2095.58±8.68.97200112.2±4.43.91500113.2±3.83.38
3-O-乙酰-16α-羟基氢化松苓新酸20107.0±7.817.30200115.3±5.14.43500110.7±8.37.45
猪苓酸C2097.92±5.75.82200106.8±4.64.29500103.9±4.74.53
齿孔酸2090.67±5.25.75200103.4±3.83.65500107.5±3.22.97
松苓新酸2097.08±9.39.54200103.8±4.74.50500104.0±2.12.02
栓菌酸2080.75±3.574.4320091.58±3.94.2950092.67±2.42.61
茯苓酸2099.08±7.77.77200103.9±3.73.5850099.63±2.32.30
3-O-乙酰基-16α-羟基松苓新酸20100.92±5.85.74200100.9±6.66.5250080.35±39.38.76
去氢茯苓酸2098.42±5.96.00200107.3±6.56.0650081.97±39.672.01
16α-羟基松苓新酸2097.83±8.68.83200107.58±3.83.53500111.47±3.12.74
土莫酸2092.58±7.98.53200116.92±3.12.68500106.4±3.23.00
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孙明月 1 , 寇金蟾 1 , 周荣贵 2 , 林佶 3
现代预防医学 | 实验技术及其应用 2024,51(2): 322-327
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现代预防医学 | 实验技术及其应用 2024, 51(2): 322-327
UPLC-Q-TOF快速定性定量检测云南省茯苓中13种三萜类化合物
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孙明月1, 寇金蟾1, 周荣贵2, 林佶3
作者信息
  • 1.大理大学公共卫生学院，云南 大理 671000
  • 2.昆明医科大学公共卫生学院
  • 3.云南省疾病预防控制中心理化实验室

    • 孙明月（1996—），女，硕士在读，研究方向：公共卫生

通讯作者:

林佶，E-mail：
Qualitative and quantitative determination of 13 triterpenoids in Wolfiporia cocos from Yunnan by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry
Ming-yue SUN1, Jin-chan KOU1, Rong-gui ZHOU2, Ji LIN3
Affiliations
  • School of Public Health, Dali University, Dali, Yunnan 671000, China
出版时间: 2024-01-25 doi: 10.20043/j.cnki.MPM.202309365
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摘要
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目的

利用超高效液相色谱-四级杆-飞行时间质谱（UPLC-Q-TOF)快速定性定量检测茯苓中13种茯苓三萜类化合物。

方法

利用超声萃取法（甲醇）对茯苓中三萜类化合物进行提取。采用ACQUITY UPLC © HSS C18柱（2.1 mm×50 mm, 1.7μm）分离,10 mmol/L乙酸铵-0.1%甲酸水溶液(A)和乙腈（B）为流动相梯度洗脱，流速为0.5 ml/min,柱温30℃,采用负离子多反应监测模式进行检测，利用精确分子量和二级质谱定性定量。

结果

13种茯苓三萜类化合物在线性范围内线性关系良好（r2≥0.99），样品加标回收率（n=6）为80.35%～116.92%，相对标准偏差为1.88%～9.7%，在茯苓药材中13种茯苓三萜类化合物均被检测出，检出量在79 433～85 900 mg/kg之间。

结论

此方法操作简便、准确、高效、灵敏，适用于茯苓药材中主要三萜类化合物的定性定量检测。

超高效液相色谱-四级杆-飞行时间质谱法  /  三萜类化合物  /  茯苓
Objective

To realize rapid qualitative and quantitative detection of 13 triterpenoids in Wolfiporia cocos from Yunnan by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry.

Methods

Triterpenoids in Wolfiporia cocos were extracted by ultrasonic extraction (methanol). The separation was carried on an ACQUITY UPLC © HSS C18 column (2.1 mm×50mm, 1.7μm) with, 10 mmol/L ammonium formate-0.1% formic acid aqueous solution and acetonitrile as mobile phase. The gradient elution flow rate was 0.5ml/min, with the column temperature of 30℃. Negative ion multiple reaction monitoring mode was used for detection. Qualitative and quantitative analysis using secondary mass spectrometry and accurate molecular weight.

Results

13 triterpenoids in Wolfiporia cocos were good with in the linear ranges (r≥0.99). The spiked recoveries were from 80.35% to 116.92%, with relative standard deviations of 1.88% to 9.7%. 13 triterpenoids were detected in Wolfiporia cocos samples, and the total contents were between 79 433-85 900 mg/kg.

Conclusion

The method is simple, accurate, efficient and sensitive, and it is suitable for the qualitative and quantitative detection of 13 triterpenoids in Wolfiporia cocos.

UPLC-Q-TOF  /  Wolfiporia cocos  /  Triterpenoids
孙明月, 寇金蟾, 周荣贵, 林佶. UPLC-Q-TOF快速定性定量检测云南省茯苓中13种三萜类化合物. 现代预防医学, 2024 , 51 (2) : 322 -327 . DOI: 10.20043/j.cnki.MPM.202309365
Ming-yue SUN, Jin-chan KOU, Rong-gui ZHOU, Ji LIN. Qualitative and quantitative determination of 13 triterpenoids in Wolfiporia cocos from Yunnan by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J]. Modern Preventive Medicine, 2024 , 51 (2) : 322 -327 . DOI: 10.20043/j.cnki.MPM.202309365
正文
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茯苓，又名茯菟、万灵桂、玉灵，归属于多孔菌科茯苓属真菌茯苓Poriacocos(Schw．)Wolf的干燥菌核，茯苓作为药食同源的传统中药[1-2]，收录于《中国药典》2020年版（一部）中，性味甘、淡、平，归心、肺、脾、肾经，是历代的中医方子里用得最多的一味中药[3-5]。云南、湖北、安徽为茯苓的传统道地产区，其中云南省茯苓品质优[2]。茯苓中三萜类化合物是主要功效成分，有增强免疫力、保肾利水、抗肿瘤等多种功效[6-11]。
茯苓中三萜类化合物的检测方法有高效液相色谱法、高效液相色谱-串联质谱法、超高效液相色谱-四级杆-飞行时间质谱法（UPLC-Q-TOF)等[12]，其中UPLC-Q-TOF可快速准确地定性定量，但现有文献只建立了茯苓酸、去氢茯苓酸等六七种物质的方法，本文建立了茯苓中13种三萜类化合物的UPLC-Q-TOF检测方法，并比较了云南省不同产地茯苓中三萜类化合物含量的差异[2,10,13-14]，为茯苓药理作用研究成分检测提供技术支持。
1　材料与方法
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1.1　材料
1.1.1　仪器
G6550 型超高效液相色谱-串联四级杆飞行时间质谱仪（安捷伦）；Nanopure 纯水机(美国 Barnstead 公司);HEIDOLPH 振荡器( 德国海道尔夫公司)；3-18K 大容量高速离心机(美国 Sigma 公司);KQ-300VDE双频数控超声波清洗器（昆山市超声仪器有限公司）。
1.1.2　试剂与材料
3-O-乙酰-16α-羟基-氢化松苓酸（CAS：168293-13-8）、松苓新酸（CAS：29220-16-4）、3-O-乙酰基-16α-羟基松苓新酸（CAS：168293-14-9）、猪苓酸C（CAS：465-18-9）、去氢茯苓酸（CAS：77012-31-8）、茯苓酸（CAS：29070-92-6）、16α-羟基松苓新酸（CAS：176390-66-2）、栓菌酸（CAS：24160-36-9，纯度≥98%）、齿孔酸（CAS：560-66-7，纯度≥94%），均购于成都乐美天医药科技有限公司；6α-羟基猪苓酸C（CAS：24513-63-1）、去氢土莫酸(CAS：6754-16-1)、3-表去氢土莫酸(CAS：167775-54-4，纯度≥98%），购于四川省维克齐生物科技有限公司；土莫酸（CAS：508-24-7，纯度≥98%），购于上海源叶生物科技有限公司；甲醇、乙醇、乙腈(色谱纯, 德国Fisher公司)；甲酸(色谱纯，纯度大于90%, 美国SIGMA-ALDRICH公司)；乙酸铵（色谱纯，DUKSAN），实验用水（18.2 MΩ.cm）。
1.1.3　样品来源
云南省茯苓主要种植区，其中普洱6件、大理6件、保山5件、楚雄3件。本次样品采集控制了茯苓的产地和部位，只采集白茯苓。
1.1.4　标准溶液配制
精密称取各标准品，加甲醇溶解并定容，配成单一标准储备液。将单一标准储备液稀释成5 μg/ml的混合标准工作液，并将混合标准工作液逐级稀释制备成约5～500 ng/ml的混合标准系列。
1.2　方法
1.2.1　色谱条件ACQUITY UPLC® HSS C18柱（2.1 mm×50 mm, 1.7 μm，美国Water公司）；进样量为2 μl，流速为0.5 ml/min,柱温为30 ℃，流动相A:0.1%甲酸-10 mmol/L乙酸铵水溶液;流动相B：乙腈；梯度洗脱程序见表1。
1.2.2　质谱条件　采用Dual AJS电喷雾电离负离子(ESI-)模式，离子源参数和特征谱库如表2和3。
1.3　样品前处理
使用高速中药粉碎机将茯苓磨成粉，过80目筛。精确称取茯苓粉0.33 g置于50 ml离心管中，用甲醇定容至10 ml,振荡20 min,使其充分混匀，超声（温度：15 ℃，频率：80 kHz）提取80 min。经10 000 r/min的离心机离心5 min后，取上层清液1 ml过0.22 μm滤膜，待测。
2　结果与讨论
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2.1　提取试剂选择
甲醇、乙醇、乙腈、纯水4种试剂代表不同的极性，纯水的极性最大，乙腈的极性最小，而13种目标化合物的极性也有强有弱，故采用4种试剂来摸索提取效率，结果显示，提取效果甲醇>乙醇>乙腈>纯水,证明甲醇的提取效果最佳，故选用100%甲醇作为提取试剂。
2.2　料液比的选择
比较了1∶10、1∶20、1∶30、1∶40和1∶50这4种料液比（固定采用纯甲醇进行提取）对茯苓的提取效率。可发现随着料液比的上升，所提取的总含量逐渐上升，在1∶30时提取的总含量达到最高。故选用1∶30作为料液比。
2.3　超声时间的选择
比较了放置20 min、超声20 min、40 min、60 min和80 min 5种超声时间对茯苓的提取效率。可发现随着超声时间的上升，提取总含量逐渐上升，在超声80 min时达到最高，考虑到工作效率的关系，超声时间没有继续增加。故选用80 min作为超声时间。
2.4　超声温度的选择
比较了15 ℃、30 ℃、45 ℃、60 ℃和75 ℃ 5种超声温度对茯苓的提取效率。可发现随着超声温度的上升，总含量逐渐下降，在15 ℃时提取含量最高。故选用15 ℃作为超声温度。
2.5　振荡时间的选择
比较了10 min、15 min、20 min、25 min和30 min 5种振荡时间对茯苓的提取效率。可发现随着振荡时间的上升，提取的总含量逐渐上升，在20 min达到最高，。故选用20 min作为振荡时间。
2.6　色谱条件优化
2.6.1　色谱柱选择
比较了ACQUITY UPLC® BEH C18柱（2.1 mm×50 mm, 1.7 μm）、ACQUITY UPLC® HSS C18柱（2.1 mm×100 mm, 1.8 μm）、ACQUITY UPLC © BEH Amide柱（2.1 mm×100 mm, 1.7 μm）、ACQUITY UPLC © HSS T3柱（2.1mm×100mm, 1.8μm）、ACQUITY UPLC © BEH HILIC柱（2.1 mm×100 mm, 1.7 μm）对目标化合物分离的影响,发现C18色谱柱能够将13种三萜类化合物全部分离出，且分离效果最佳,但ACQUITY UPLC® BEH C18柱（2.1 mm×50 mm, 1.7 μm）分离的目标化合物峰型更好，故选用C18色谱柱（2.1 mm×50 mm, 1.7 μm）。
2.6.2　流动相选择
在优选流动相时，选择了0.1%甲酸水-甲醇、0.1%甲酸水-乙腈作比较，发现乙腈作为有机相时，可以分离出全部目标化合物，但峰形不太理想。之后再选用5 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈、纯水-乙腈、0.1%氨水-乙腈、10 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈进行比较。发现5 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈和10 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈为流动相时，均可分离出13种目标化合物，但只有10 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈的响应值高峰形较好，且无杂峰，故选用10 mmol/L乙酸铵-0.1%甲酸水溶液-乙腈为流动相。
2.6.3　流动相梯度确定
通过确定色谱柱和流动相，目标化合物分离程度及响应值可，但峰形不太理想，通过调整洗脱梯度，使目标化合物的峰形理想，确定了最终的流动相梯度，见表4。
综合使用以上色谱条件和质谱条件，得到13种三萜类化合物的标准色谱图（图1）和质谱图（图2）。
2.7　质谱条件优化
2.7.1　一级质谱参数的优化
采用Dual AJS电喷雾电离负离子(ESI-)模式,MS采样模式，对所有标准品进行检测。首先对离子源参数进行优化，经反复试验得出最优的离子源参数如表3，利用一级质谱条件，利用13种三萜类化合物的保留时间和精确质量数建好的特征谱库，对标准品溶液进行定性。调整保留时间偏差<0.1 min和质量偏差<5 ppm。在比对[M-H]-、[M+Cl]-、[M+Br]-等几种分子离子峰, 发现[M-H]-峰的灵敏度最高且稳定，因此选择[M-H]-作为定量离子。选择使用 Agile 积分器。离子源参数不变。应用以上设置对13种目标化合物进行一级筛查,能够找到全部化合物,化合物响应信号强且峰形好,表明以上参数为最优参数,得到一级质谱图。
2.7.2　二级质谱参数的优化
保留一级质谱下的最优参数，选择Targeted MS/MS采样模式，在Targeted List输入在一级模式得出的目标化合物的保留时间和精确质量数。通过不断调整碰撞电压和ISO.Width，选择使用 MS/MS 积分器，得出母离子相对丰度较低且响应稳定、而碎片离子相对丰度较高，杂质离子干扰少的二级质谱图,相对应的电压则为最优碰撞电压。最终确定ISO.Width为Narrow(～1.3m/z)，13种三萜类化合物的最优碰撞电压及碎片离子见表3。
2.8　方法学考察
2.8.1　线性范围、检出限与定量限
在5～500 ng/ml 的线性范围内, 13种三萜类化合物的线性方程、相关系数、检出限和定量限见表5。方法的相关系数在0.991 2～0.999 6之间。用各物质的最低浓度点进样，以3倍信噪比计算出检出限，以10倍信噪比计算出定量限。
2.8.2　稳定性
将浓度100 ng/ml的标准混合液分别在2、4、6、8、10、12、14、16、18、20、22、24、48h时进行检测，RSD均小于5.27%，说明标准品溶液在48 h内稳定，见表5。
2.8.3　加标回收率
以空白样品为基质，进行低、中、高三种浓度（20、200、500 ng/ml）的6份加标实验。计算得出方法的加标回收率及其相对标准偏差（RSD），见表6。
2.9　实际样品检测
将采购的茯苓粉过80目筛，充分混匀。按本法进行处理测定，茯苓药材中13种三萜类化合物均被检测出，其中茯苓酸的含量最高，其次为松苓新酸。楚雄、大理、保山、普洱4个地州的茯苓样品三萜酸化合物总含量均值分别为85 900 mg/kg>84 240 mg/kg>82 017 mg/kg>79 433 mg/kg。样品色谱图见图3。
3　结论
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本研究通过优化色谱条件和质谱条件，建立了UPLC-Q-TOF检测茯苓中13种三萜类物质的快速定性定量方法，其线性关系、精密度、稳定性、回收率良好，可高效、快速、准确检测茯苓样品中三萜类化合物。13种三萜类化合物在6 min内可全部洗脱出来，其峰形和分离效果良好，有效地缩短了检测时间。本文还比较了云南省楚雄、大理、保山、普洱4个地州茯苓样品三萜酸化合物的总含量，发现不同产地对茯苓三萜类化合物含量有一定的影响。
基金
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  • 云南省教育厅科学研究基金项目(2023Y0944)
文献
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2024年第51卷第2期
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doi: 10.20043/j.cnki.MPM.202309365
  • 接收时间：2023-09-19
  • 首发时间：2026-03-19
  • 出版时间：2024-01-25
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  • 收稿日期：2023-09-19
基金
云南省教育厅科学研究基金项目(2023Y0944)
作者信息
    1.大理大学公共卫生学院，云南 大理 671000
    2.昆明医科大学公共卫生学院
    3.云南省疾病预防控制中心理化实验室

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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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