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Article(id=1239238142163735129, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239238136711139764, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2023-0741, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1700409600000, receivedDateStr=2023-11-20, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773386997023, onlineDateStr=2026-03-13, pubDate=1722355200000, pubDateStr=2024-07-31, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773386997023, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773386997023, creator=13701087609, updateTime=1773386997023, updator=13701087609, issue=Issue{id=1239238136711139764, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='7', pageStart='1105', pageEnd='1284', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773386995723, creator=13701087609, updateTime=1773387118529, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239238651851370909, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239238136711139764, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239238651851370910, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239238136711139764, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1169, endPage=1175, ext={EN=ArticleExt(id=1239238142402810473, articleId=1239238142163735129, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Determination of vitamin D3 in vitamin D drops by high resolution sampling two-dimensional chromatography, columnId=1239148838318043851, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Ingredient Analys, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish an innovative analytical method based on high resolution sampling two-dimensional chromatography (HiRes 2D-LC) for determination of the content of vitamin D3 in vitamin D drops.

Methods:

Two-dimensional liquid chromatography was used. Thermo HYPERSIL Gold Silica (100 mm×2.1 mm, 1.9 μm) column was used in the first dimension with n-hexane-n-amyl alcohol (996∶4) as mobile phase. The flow rate was 0.2 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. In the second dimension liquid chromatography, ShimPack Velox Hilic (50 mm×2.1 mm, 2.7 μm) was used as the column with n-hexane-n-pentanol-isopropanol (98∶1∶1) as the mobile phase. The flow rate was 0.5 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. A six-position 14-way valve and was equipped with 2 multi-center cutting valves was equipped to make multiple consecutive cuts of the pre-vitamin D3 peak and vitamin D3 peak.

Results:

The calibration curves showed a good linearity at the range of 1.018 4-5.092 mg·mL-1 (r≥0.999 8). The precision test showed the RSDs of the peak area of pre-vitamin D3 and vitamin D3 were 0.95% and 0.40%, respectively. The repeatability test showed the RSD of vitamin D3 content was 0.41%. The average recovery rate (n=9) was 101.4%. The test solution was stable at 4 ℃ and 10 ℃ for 12 h, and the RSDs were 0.58% and 0.66%, respectively. The contents of vitamin D3 in the samples of vitamin D drops measured by this method were 100.4%, 101.6%, 100.9%, 101.6%, 102.7% and 101.6%, which was basically consistent with the results measured by the fourth method in General Chapter 0722 of ChP 2020 Vol Ⅳ.

Conclusion:

This method has a good specificity and high sensitivity to accurately determine the content of vitamin D3 in vitamin D drops.

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目的：

建立高分辨采样二维液相色谱法（HiRes 2D-LC）对维生素D滴剂中维生素D3进行准确定量分析。

方法：

第一维液相色谱采用Thermo HYPERSIL Gold Silica（100 mm×2.1 mm，1.9 μm）色谱柱，以正己烷-正戊醇（996∶4）为流动相，流速0.2 mL·min-1，检测波长265 nm，柱温40 ℃；第二维液相色谱采用ShimPack Velox Hilic（50 mm×2.1 mm，2.7 μm）色谱柱，以正己烷-正戊醇-异丙醇（98∶1∶1）为流动相，流速0.5 mL·min-1，检测波长265 nm，柱温40 ℃。二维接口采用六位十四通阀，并配置2个多中心切割阀，对前维生素D3峰和维生素D3峰进行多次连续切割。

结果：

维生素D3质量浓度在1.018 4~5.092 mg·mL-1范围内线性关系良好（r≥0.999 8），前维生素D3和维生素D3精密度试验RSD分别为0.95%和0.40%，重复性试验RSD为0.41%，平均加标回收率为101.4%。供试品溶液在4 ℃和10 ℃放置12 h稳定，RSD分别为0.58%、0.66%。采用本法测得6批维生素D滴剂样品中维生素D3的含量分别为100.4%、101.6%、100.9%、101.6%、102.7%、101.6%，与采用2020年版《中华人民共和国药典》四部通则0722第四法所测结果基本一致。

结论：

本方法具有优异的灵敏度、重复性和定量准确性，且省去烦琐的样品前处理步骤，缩短分析时间，改善长样品环带来的峰展宽等问题，显著提高了维生素D3的含量测定效率，降低分析成本，为维生素D滴剂等主成分与辅料难分离制剂的准确定量提供新方法。

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Tel：（0592）5619836；E-mail：

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Drug Stand China， 2020， 21(2)： 107, articleTitle=Investigation on the calculation methods of vitamin D assay by HPLC, refAbstract=null)], funds=[Fund(id=1239238154692120696, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, awardId=XMSJ202305, language=CN, fundingSource=* 厦门市市场监督管理局科技计划项目(XMSJ202305), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239238146752303925, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, xref=1., ext=[AuthorCompanyExt(id=1239238146756498231, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, companyId=1239238146752303925, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.Xiamen Institute for Food and Drug Quality Control, Xiamen 361012, China), AuthorCompanyExt(id=1239238146764886839, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, companyId=1239238146752303925, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.厦门市食品药品质量检验研究院，厦门 361012)]), AuthorCompany(id=1239238146848772923, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, xref=2., ext=[AuthorCompanyExt(id=1239238146857161532, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, companyId=1239238146848772923, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.Sinopharm Xingsha Pharmaceuticals (Xiamen) Co., Ltd., Xiamen 361026, China), AuthorCompanyExt(id=1239238146865550141, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, companyId=1239238146848772923, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.国药控股星鲨制药（厦门）有限公司，厦门 361026)])], figs=[ArticleFig(id=1239238151131156489, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=EN, label=Fig.1, caption=2D chromatogram of correction factor f2 standard solution (pre-vitamin D3), figureFileSmall=HoHUqe9J1nmlJad1Y5yoRw==, figureFileBig=qS+ghLfMWtiIGXcdVWrJrQ==, tableContent=null), ArticleFig(id=1239238151206653967, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=CN, label=图1, caption=校正因子f2对照品溶液第二维高效液相色谱图(前维生素D3)

A.空白溶剂(blank solvent)　B.空白辅料溶液（blank excipient solution）　C.校正因子f2对照品溶液(correction factor f2 standard solution) D.供试品溶液(sample solution)

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A.空白溶剂(blank solvent)　B.空白辅料溶液（blank excipient solution） C.校正因子f2溶液(correction factor f2 standard solution)　D.供试品溶液(sample solution)

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Sampling time

, figureFileSmall=null, figureFileBig=null, tableContent=
采样时间
(sampling time)/s		模式
(mode)		第一维切割开始时间
(1D cut start time)/min		第二维运行开始时间
(2D run start time)/min		样品仓
(deck)		样品环
(loop)
9.60Time6.8510.64A2
9.60Time7.019.64A3
9.60Time7.178.64A4
9.60Time7.337.64A5
9.60Time12.0517.00B2
9.60Time12.2116.00B3
9.60Time12.3715.00B4
9.60Time12.5314.00B5
9.60Time12.6913.00B6
9.60Time12.8523.00A1
9.60Time13.0122.00A2
9.60Time13.1721.00A3
9.60Time13.3320.00A4
9.60Time13.4919.00A5
), ArticleFig(id=1239238152313950282, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=CN, label=表1, caption=

采样时间

, figureFileSmall=null, figureFileBig=null, tableContent=
采样时间
(sampling time)/s		模式
(mode)		第一维切割开始时间
(1D cut start time)/min		第二维运行开始时间
(2D run start time)/min		样品仓
(deck)		样品环
(loop)
9.60Time6.8510.64A2
9.60Time7.019.64A3
9.60Time7.178.64A4
9.60Time7.337.64A5
9.60Time12.0517.00B2
9.60Time12.2116.00B3
9.60Time12.3715.00B4
9.60Time12.5314.00B5
9.60Time12.6913.00B6
9.60Time12.8523.00A1
9.60Time13.0122.00A2
9.60Time13.1721.00A3
9.60Time13.3320.00A4
9.60Time13.4919.00A5
), ArticleFig(id=1239238152460750931, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=EN, label=Tab.2, caption=

f1 correction factor measurement results

, figureFileSmall=null, figureFileBig=null, tableContent=
对照品量(mass of reference substance)/g维生素D3峰面积(peak area of vitamin D3)f1平均值(average value)RSD/%
0.025 46724.93.512 2×10-33.517 3×10-31.2
0.025 91745.13.477 4×10-3
0.025 30710.23.562 4×10-3
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f1校正因子测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
对照品量(mass of reference substance)/g维生素D3峰面积(peak area of vitamin D3)f1平均值(average value)RSD/%
0.025 46724.93.512 2×10-33.517 3×10-31.2
0.025 91745.13.477 4×10-3
0.025 30710.23.562 4×10-3
), ArticleFig(id=1239238152674660445, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=EN, label=Tab.3, caption=

f2 correction factor measurement results

, figureFileSmall=null, figureFileBig=null, tableContent=
对照品量
(mass of reference substance)/g		前维生素D3峰面积
(peak area of pre-vitamin D3)		维生素D3峰面积
(peak area of vitamin D3)		f2平均值
(average value)		RSD/%
0.025 4695.7548.06.606 1×10-36.656 2×10-30.77
0.025 9197.4554.86.709 0×10-3
0.025 3093.1529.06.653 4×10-3
), ArticleFig(id=1239238152766935138, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=CN, label=表3, caption=

f2校正因子测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
对照品量
(mass of reference substance)/g		前维生素D3峰面积
(peak area of pre-vitamin D3)		维生素D3峰面积
(peak area of vitamin D3)		f2平均值
(average value)		RSD/%
0.025 4695.7548.06.606 1×10-36.656 2×10-30.77
0.025 9197.4554.86.709 0×10-3
0.025 3093.1529.06.653 4×10-3
), ArticleFig(id=1239238152926318694, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=EN, label=Tab.4, caption=

Recovery test results of vitamin D3

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加入量
(added amount)/μg		测得量
(measured amount)/μg		回收率
(recovery)/%		均值
(average value)/%		RSD/%平均回收率
(average recovery)/%		RSD/%
21.8621.932100.3101.00.66101.40.59
20.5420.717100.9
20.2220.556101.7
25.6826.011101.3101.40.18
25.6225.983101.4
24.8425.250101.6
31.3631.721101.2101.90.66
31.0631.829102.5
31.1831.689101.6
), ArticleFig(id=1239238153022787691, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=CN, label=表4, caption=

维生素D3回收率试验结果

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加入量
(added amount)/μg		测得量
(measured amount)/μg		回收率
(recovery)/%		均值
(average value)/%		RSD/%平均回收率
(average recovery)/%		RSD/%
21.8621.932100.3101.00.66101.40.59
20.5420.717100.9
20.2220.556101.7
25.6826.011101.3101.40.18
25.6225.983101.4
24.8425.250101.6
31.3631.721101.2101.90.66
31.0631.829102.5
31.1831.689101.6
), ArticleFig(id=1239238153127645296, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=EN, label=Tab.5, caption=

Assay results

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批号
(batch number)		每粒含维生素D3/单位
(vitamin D3 content per drop)/U		含量(content)/%
本法
(studied method)		2020年版《中国药典》四部通则0722四法
(the forth method of General Chapter 0722 of ChP 2020 Vol Ⅳ)
129231014400100.4100.7
129224259101.6101.2
129224232100.9101.2
129224064101.6101.8
129224052102.7102.4
129231233101.6101.7
), ArticleFig(id=1239238154574680180, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239238142163735129, language=CN, label=表5, caption=

含量测定结果表

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批号
(batch number)		每粒含维生素D3/单位
(vitamin D3 content per drop)/U		含量(content)/%
本法
(studied method)		2020年版《中国药典》四部通则0722四法
(the forth method of General Chapter 0722 of ChP 2020 Vol Ⅳ)
129231014400100.4100.7
129224259101.6101.2
129224232100.9101.2
129224064101.6101.8
129224052102.7102.4
129231233101.6101.7
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高分辨采样二维液相色谱法测定维生素D滴剂中维生素D3含量研究*
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吴珏 1 , 郭伟斌 1 , 邱晓峰 2 , 郑淑凤 1
药物分析杂志 | 成分分析 2024,44(7): 1169-1175
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药物分析杂志 | 成分分析 2024, 44(7): 1169-1175
高分辨采样二维液相色谱法测定维生素D滴剂中维生素D3含量研究*
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吴珏1 , 郭伟斌1, 邱晓峰2, 郑淑凤1
作者信息
  • 1.厦门市食品药品质量检验研究院，厦门 361012
  • 2.国药控股星鲨制药（厦门）有限公司，厦门 361026

    • Tel：（0592）5619836；E-mail：

Determination of vitamin D3 in vitamin D drops by high resolution sampling two-dimensional chromatography
Jue WU1 , Wei-bin GUO1, Xiao-feng QIU2, Shu-feng ZHENG1
Affiliations
  • 1.Xiamen Institute for Food and Drug Quality Control, Xiamen 361012, China
  • 2.Sinopharm Xingsha Pharmaceuticals (Xiamen) Co., Ltd., Xiamen 361026, China
出版时间: 2024-07-31 doi: 10.16155/j.0254-1793.2023-0741
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摘要
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目的：

建立高分辨采样二维液相色谱法（HiRes 2D-LC）对维生素D滴剂中维生素D3进行准确定量分析。

方法：

第一维液相色谱采用Thermo HYPERSIL Gold Silica（100 mm×2.1 mm，1.9 μm）色谱柱，以正己烷-正戊醇（996∶4）为流动相，流速0.2 mL·min-1，检测波长265 nm，柱温40 ℃；第二维液相色谱采用ShimPack Velox Hilic（50 mm×2.1 mm，2.7 μm）色谱柱，以正己烷-正戊醇-异丙醇（98∶1∶1）为流动相，流速0.5 mL·min-1，检测波长265 nm，柱温40 ℃。二维接口采用六位十四通阀，并配置2个多中心切割阀，对前维生素D3峰和维生素D3峰进行多次连续切割。

结果：

维生素D3质量浓度在1.018 4~5.092 mg·mL-1范围内线性关系良好（r≥0.999 8），前维生素D3和维生素D3精密度试验RSD分别为0.95%和0.40%，重复性试验RSD为0.41%，平均加标回收率为101.4%。供试品溶液在4 ℃和10 ℃放置12 h稳定，RSD分别为0.58%、0.66%。采用本法测得6批维生素D滴剂样品中维生素D3的含量分别为100.4%、101.6%、100.9%、101.6%、102.7%、101.6%，与采用2020年版《中华人民共和国药典》四部通则0722第四法所测结果基本一致。

结论：

本方法具有优异的灵敏度、重复性和定量准确性，且省去烦琐的样品前处理步骤，缩短分析时间，改善长样品环带来的峰展宽等问题，显著提高了维生素D3的含量测定效率，降低分析成本，为维生素D滴剂等主成分与辅料难分离制剂的准确定量提供新方法。

高分辨采样  /  二维液相色谱法  /  正相色谱法  /  维生素D滴剂  /  前维生素D3  /  维生素D3  /  含量测定  /  峰纯度确证
Objective:

To establish an innovative analytical method based on high resolution sampling two-dimensional chromatography (HiRes 2D-LC) for determination of the content of vitamin D3 in vitamin D drops.

Methods:

Two-dimensional liquid chromatography was used. Thermo HYPERSIL Gold Silica (100 mm×2.1 mm, 1.9 μm) column was used in the first dimension with n-hexane-n-amyl alcohol (996∶4) as mobile phase. The flow rate was 0.2 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. In the second dimension liquid chromatography, ShimPack Velox Hilic (50 mm×2.1 mm, 2.7 μm) was used as the column with n-hexane-n-pentanol-isopropanol (98∶1∶1) as the mobile phase. The flow rate was 0.5 mL·min-1. The samples were injected and tested at the wavelength of 265 nm. The column temperature was 40 ℃. A six-position 14-way valve and was equipped with 2 multi-center cutting valves was equipped to make multiple consecutive cuts of the pre-vitamin D3 peak and vitamin D3 peak.

Results:

The calibration curves showed a good linearity at the range of 1.018 4-5.092 mg·mL-1 (r≥0.999 8). The precision test showed the RSDs of the peak area of pre-vitamin D3 and vitamin D3 were 0.95% and 0.40%, respectively. The repeatability test showed the RSD of vitamin D3 content was 0.41%. The average recovery rate (n=9) was 101.4%. The test solution was stable at 4 ℃ and 10 ℃ for 12 h, and the RSDs were 0.58% and 0.66%, respectively. The contents of vitamin D3 in the samples of vitamin D drops measured by this method were 100.4%, 101.6%, 100.9%, 101.6%, 102.7% and 101.6%, which was basically consistent with the results measured by the fourth method in General Chapter 0722 of ChP 2020 Vol Ⅳ.

Conclusion:

This method has a good specificity and high sensitivity to accurately determine the content of vitamin D3 in vitamin D drops.

high resolution sampling  /  two-dimensional chromatography  /  normal plase chromatography  /  vitamin D drops  /  pre-vitamin D3  /  vitamin D3  /  normal-phase chromatography  /  peak purity confirmation
吴珏, 郭伟斌, 邱晓峰, 郑淑凤. 高分辨采样二维液相色谱法测定维生素D滴剂中维生素D3含量研究*. 药物分析杂志, 2024 , 44 (7) : 1169 -1175 . DOI: 10.16155/j.0254-1793.2023-0741
Jue WU, Wei-bin GUO, Xiao-feng QIU, Shu-feng ZHENG. Determination of vitamin D3 in vitamin D drops by high resolution sampling two-dimensional chromatography[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (7) : 1169 -1175 . DOI: 10.16155/j.0254-1793.2023-0741
正文
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维生素D是类固醇类衍生物，市售制剂主要有维生素D软胶囊、维生素D滴剂等，其主要成分为维生素D3或维生素D2，辅料为植物油、明胶、甘油等。在临床上主要用于预防和治疗维生素D缺乏性佝偻病、骨质疏松症，长期超剂量摄入可能会引起高钙血症、钙沉积引起的肌肉乏力、关节疼痛、弥漫性骨质脱矿化等中毒现象[1]。
2020年版《中华人民共和国药典》（简称《中国药典》）收载了4种维生素D的含量测定方法[2]，前三法均需对供试品进行皂化回流等前处理，第四法采用柱切换二维液相色谱法，将前维生素D峰和维生素D峰切入收集管中，再注入第二维色谱系统进行分析，存在分析时间长，峰展宽等问题。此外，相关文献显示，对于口服液[3]、片剂[4-5]等无油性辅料干扰的制剂，可采用反相液相色谱法进行分析。采用HPLC-MS法对维生素AD滴剂中维生素D3的含量进行测定，仍存在固相萃取等复杂前处理步骤[6-7]。
近年来，不论是全二维液相色谱法还是中心切割二维液相色谱法，二维液相色谱技术被广泛应用于多组分同步测定、微量杂质分析等领域，但均常见于定性分析[8]及微量成分定量研究[9-11]，缺乏主成分等常量样品的定量研究。中心切割二维液相色谱法中，多中心切割技术可针对多个目标峰进行切割，且通过高分辨采样可进行多次连续切割以解决峰容量大的问题[12]，从而对目标物质进行定量分析。
本研究开发了一种高分辨采样二维液相色谱方法，通过多中心切割阀对第一维色谱图中的前维生素D3和维生素D3 2个目标峰进行多次连续切割并利用多组小体积样品环不间断收集，将第一维中2个目标峰完整注入第二维液相系统，实现目标组分与油性辅料的分离和准确定量。本方法无需烦琐的样品前处理步骤，缩短分析时间，改善长样品环带来的峰展宽等问题，显著提高了维生素D3的含量测定效率，降低分析成本，为维生素D滴剂等主成分与辅料难分离制剂的准确定量提供新方法。
1　仪器与试药
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1290 infinity Ⅱ二维液相色谱系统(安捷伦科技有限公司)，配备六位十四通阀、2个多中心切割阀(配置的样品环体积为40 μL)、VWD检测器、DAD检测器；XSE205十万分之一电子分析天平(METTLER TOLEDO公司)；HH-2数显恒温水浴锅(常州国华电器有限公司)；XM-500VDE三频超声波清洗机(小美超声仪器昆山有限公司)。
正己烷、正戊醇、异辛烷(均为色谱纯，上海阿拉丁生化科技股份有限公司)；异丙醇(色谱纯，默克股份两合公司)；2，6-二叔丁基对甲酚(化学纯，中国医药集团上海化学试剂公司)；大豆油(空白辅料，由生产企业提供)；维生素D3对照品(批号100061-202311，中国食品药品检定研究院，含量100.0%)；维生素D滴剂(软胶囊型，批号129231014、129224259、129224232、129224064、129224052，129231233，每粒400单位)。试验用水均为超纯水，由Milli-Q超纯水系统制备。
2　方法与结果
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2.1　溶液制备
2.1.1　供试品溶液
取维生素D滴剂内容物适量(约含维生素D3 1 000单位)，精密称定，置10 mL棕色量瓶中，用正己烷溶解并稀释至刻度，摇匀，即得。
2.1.2　对照品储备溶液
取维生素D3对照品约25 mg，精密称定，置100 mL棕色量瓶中，加异辛烷80 mL，避免加热，超声处理1 min使完全溶解，用异辛烷稀释至刻度，摇匀，精密量取5 mL，置50 mL棕色量瓶中，用异辛烷稀释至刻度，摇匀，即得。
2.1.3　校正因子对照品溶液
校正因子f1对照品溶液：精密量取对照品储备溶液5 mL，置50 mL棕色量瓶中，用正己烷稀释至刻度，摇匀，即得。
校正因子f2对照品溶液：精密量取对照品储备溶液5 mL，置50 mL棕色量瓶中，加2，6-二叔丁基对甲酚结晶1粒，通氮排除空气后，密塞，置90 ℃水浴中加热1.5 h，取出，迅速冷却，用正己烷稀释至刻度，摇匀，即得。
2.1.4　空白辅料溶液
精密称取大豆油约0.6 g，置10 mL棕色量瓶中，用正己烷溶解并稀释至刻度，摇匀，即得。
2.2　色谱条件
第一维液相色谱采用Thermo HYPERSIL Gold Silica (100 mm×2.1 mm，1.9 μm)色谱柱，以正己烷-正戊醇(996∶4)为流动相，流速0.2 mL·min-1，检测波长265 nm，柱温40 ℃，进样体积10 μL。
第二维液相色谱采用ShimPack Velox Hilic (50 mm×2.1 mm，2.7 μm)色谱柱，以正己烷-正戊醇-异丙醇(98∶1∶1)为流动相，流速0.5 mL·min-1，检测波长265 nm，柱温40 ℃。通过阀切换采用高分辨采样，前维生素D3目标峰切割开始时间6.85 min，采样时间9.6 s，连续采集4次。维生素D3目标峰切割开始时间为12.05 min，采样时间9.6 s，连续采集10次，采样时间见表1。
2.3　含量计算方法
维生素D3总量Ci=f1Ai1+f2Ai2，式中Ai1为维生素D3峰面积，Ai2为前维生素D3峰面积。
维生素D3百分标示含量= Ci×平均装量×稀释倍数/(取样量×0.025×标示量)，维生素D3滴剂以单位表示维生素D3的总量，每单位相当于维生素D3 0.025 μg。
2.4　方法学验证
2.4.1　专属性试验
精密量取供试品溶液、校正因子f2对照品溶液、空白辅料溶液、空白溶剂（正己烷）各10 μL，分别按“2.2”项下条件进样测定。结果见图1、2所示，空白辅料大豆油和溶剂正己烷对前维生素D3峰和维生素D3峰均无干扰。
2.4.2　精密度试验
精密量取校正因子f2对照品溶液10 μL，按“2.2”项下条件连续进样6次，前维生素D3峰面积和维生素D3峰面积的RSD分别为0.95%和0.40%。
2.4.3　重复性试验
取维生素D滴剂内容物(分别相当于维生素D3 800、1 000、1 200单位)各3份，精密称定，按“2.1.1”项下方法制备供试品溶液，按“2.2”项下条件测定，按“2.3”项下公式计算9份样品中维生素D3的平均含量为100.4%，RSD为0.41%。
2.4.4　线性关系考察
精密量取对照品储备溶液2、4、5、6、8、10 mL，分别置50 mL棕色量瓶中，用正己烷稀释至刻度，摇匀，滤过，取续滤液按“2.2”项下方法测定。以维生素D3质量浓度(C)为横坐标，维生素D3峰面积(A)为纵坐标，进行线性回归，得维生素D3回归方程
表明维生素D3质量浓度在1.018 4~5.092 μg·mL-1范围内与峰面积呈良好的线性关系。
2.4.5　校正因子测定
精密量取校正因子f1对照品溶液10 μL，按“2.2”项下条件进样测定，计算校正因子f1，f1=C1/A1，式中C1为维生素D3对照品溶液浓度，A1为色谱图中维生素D3峰面积。
精密量取校正因子f2对照品溶液10 μL，按“2.2”项下条件进样测定，计算校正因子f2，f2=(C1-f1A1)/A2，式中C1为f1测定时维生素D3对照品溶液的浓度，f1为维生素D3校正因子，A1为色谱图中维生素D3峰面积，A2为色谱图中前维生素D3峰面积。
测定结果如表2、3所示。
2.4.6　稳定性试验
鉴于试验过程中可能存在由测定时间长等原因引起的样品不能及时分析的情况，本试验考察样品在4和10 ℃下的稳定性。取供试品溶液于4 ℃放置0、2、4、8、12 h，另取供试品溶液于10 ℃放置0、2、4、8、12 h，分别按“2.2”项下条件测定，结果显示4和10 ℃放置的各供试品溶液峰面积RSD分别为0.58%和0.66%，表明供试品溶液在4和10 ℃稳定性良好。
2.4.7　回收率试验
精密称取维生素D3对照品约10、12.5、15 mg各3份，分别置100 mL棕色量瓶中，加异辛烷溶解并稀释至刻度，摇匀，精密量取5 mL，置50 mL量瓶中，加正己烷稀释至刻度，摇匀，精密量取2 mL，置10 mL量瓶中，再分别加入空白辅料适量(根据制剂处方各加入约1粒量)，用正己烷溶解并稀释至刻度，摇匀，滤过，精密量取续滤液10 μL，按“2.2”项下条件测定，按“2.3”项下公式计算回收率(表4)，结果表明回收率良好。
2.4.8　耐用性试验
2.4.8.1　流动相流速
调节第一维流速分别为0.15、0.2、0.3 mL·min-1，当流速为0.15 mL·min-1时第一维色谱图中维生素D3峰峰宽较大，不能将其完全切割转移到第二维以实现准确定量；当流速为0.2 mL·min-1时，前维生素D3峰与维生素D3峰均可完全切割进入第二维；当流速为0.3 mL·min-1时，前维生素D3峰与辅料峰大部分重叠难以确定切割开始时间。设置第一维流速为0.2 mL·min-1，调节第二维流速分别为0.4、0.5、0.6 mL·min-1，第二维色谱表现无明显差别。
2.4.8.2　流动相比例
改变第一维流动相正己烷-正戊醇的比例分别为997∶3、996∶4和995∶5，仅对保留时间存在影响，正己烷-正戊醇为995∶5时，前维生素D3峰与辅料峰分离度相对较差；设置第一维流动相为正己烷-正戊醇996∶4，只调整第二维流动相正己烷-正戊醇-异丙醇比例分别为99∶0.5∶0.5、98∶1∶1和97∶1.5∶1.5，第二维色谱各峰仅在保留时间上存在细微差别。
2.4.8.3　不同色谱柱
分别以Thermo HYPERSIL Gold Silica(100 mm×2.1 mm，1.9 μm)色谱柱和ShimPack Velox Hilic(100 mm×2.1 mm，2.7 μm)色谱柱作为第一维色谱柱，结果采用ShimPack Velox Hilic(100 mm×2.1 mm，2.7 μm)色谱柱时第一维色谱图中前维生素D3峰与辅料峰不能较好分离，影响切割开始时间的判断。
2.5　样品含量测定
精密量取“2.1.1”项下供试品溶液10 μL，照“2.2”项下条件测定，按“2.3”项下公式计算维生素D3含量。结果如表5所示，6批样品的含量测定结果与《中国药典》通则0722四法测得结果基本一致。色谱图见图3~5。
3　讨论
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本研究采用多中心切割二维液相色谱法对维生素D滴剂进行定量研究，相较于药典及文献报道的二维液相色谱方法[13]，将分析时间由2020年版《中国药典》四部通则0722四法的70 min缩短至25 min，提高了分析效率，降低了检验成本，且解决了长样品环带来的峰展宽等问题。当样品浓度与药典方法一致时，进样量仅为药典方法的1/10，提高了检测灵敏度，可为微量样品的测定提供参考。
《中国药典》及文献报道的一维液相色谱方法中，样品需经皂化回流、氮吹复溶[14]、超声离心[15-16]等前处理，操作烦琐，易造成测定成分的损失。本研究采用正己烷直接溶解样品，降低了样品前处理过程中对设备和人工的要求，操作简便，极大缩短了前处理时间。
从二维液相色谱峰中提取前维生素D3和维生素D3的光谱图，样品与对照品光谱吸收特征一致，进一步表明2个定量峰与辅料之间实现了完全分离，使用本方法所测定的维生素D3含量准确、可靠。
文献报道了4种维生素D含量的计算方法[17]，且其计算结果存在一定差异。本研究参考《中国药典》，通过加热破坏维生素D3对照品溶液，使仅产生前维生素D3峰，未产生其他杂质峰，计算获得前维生素D3的相对校正因子，维生素D3总量以维生素D3与前维生素D3含量之和计，可有效反映维生素D3的实际含量。
4　结论
收起
本研究建立高分辨采样二维液相色谱法对维生素D滴剂中维生素D3含量进行测定，可以实现目标成分的完全分离和准确定量，该技术可为难分离样品的定量分析提供参考。
基金
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  • * 厦门市市场监督管理局科技计划项目(XMSJ202305)
文献
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2024年第44卷第7期
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doi: 10.16155/j.0254-1793.2023-0741
  • 接收时间：2023-11-20
  • 首发时间：2026-03-13
  • 出版时间：2024-07-31
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  • 收稿日期：2023-11-20
基金
* 厦门市市场监督管理局科技计划项目(XMSJ202305)
作者信息
    1.厦门市食品药品质量检验研究院，厦门 361012
    2.国药控股星鲨制药（厦门）有限公司，厦门 361026
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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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