超高效液相色谱-串联质谱法同时测定化妆品中100种糖皮质激素

doi:10.3724/SP.J.1123.2024.03011

摘要/Abstract

摘要：

我国《化妆品安全技术规范》(2015年版)规定糖皮质激素为化妆品中禁用原料。本论文建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测化妆品中100种非法添加糖皮质激素的分析方法,涵盖了现行国家标准GB/T 24800.2-2009、GB/T 40145-2021和《化妆品安全技术规范》(2015年版)中列出的58种糖皮质激素,以及42种新型糖皮质激素,其中包含2种迄今未见文献报道的糖皮质激素美替诺龙醋酸酯和地塞米松9,11-环氧。样品用含0.2%(v/v)乙酸的饱和氯化钠溶液分散,用含0.2%(v/v)乙酸的乙腈提取,向乙腈提取液中加入等体积水析出非极性杂质,再加入10%(质量分数)亚铁氰化钾溶液和20%(质量分数)乙酸锌溶液(含0.4%(v/v)乙酸)作为沉淀剂进一步净化,选用Waters ACQUITY UPLC BEH C₁₈色谱柱(150 mm×3.0 mm, 1.7 μm)进行色谱分离,以0.2%(v/v)乙酸水溶液-0.2%(v/v)乙酸甲醇溶液为流动相梯度洗脱。在电喷雾正离子模式下以动态多反应监测方式(MRM)测定,外标法定量。以MRM-信息依赖采集-增强子离子扫描模式(MRM-IDA-EPI)得到的增强子离子质谱图(EPI)进行阳性样品确证。结果显示:100种糖皮质激素在2.5~60 ng/mL范围内具有良好的线性关系,相关系数均大于0.99,除环索奈德在膏霜乳基质中出现基质抑制效应以外,其余99种糖皮质激素均无明显的基质效应。所有目标物的方法检出限和定量限分别为0.03 μg/g和0.1 μg/g。在3个不同的添加水平下(1倍、2倍和8倍定量限),水基质中目标化合物的回收率为79.6%~114.4%, RSD为0.7%~9.4%(n=6),膏霜乳基质中目标化合物的回收率为79.5%~112.1%, RSD为0.7%~12.9%(n=6)。筛查了47种实际样品,在3个阳性样品中检出了5种糖皮质激素,并用MRM-IDA-EPI进行了确证。本检测方法操作简便、高效,适用于化妆品中100种糖皮质激素的快速筛查和测定,可填补化妆品中糖皮质激素的监管空白,为化妆品的质量监管提供了有力的技术手段。

关键词: 超高效液相色谱-串联质谱, 糖皮质激素, 化妆品, 非法添加

Abstract:

Adding glucocorticoids to cosmetics is strictly prohibited under Safety and Technical Specification for Cosmetics (2015) regulations. Accordingly, a method for simultaneously determining 100 glucocorticoids in cosmetics using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Apart from the 58 glucocorticoids listed in the two current national standards (GB/T 24800.2-2009 and GB/T 40145-2021) and the Safety and Technical Specification for Cosmetics (2015) regulations, 42 new glucocorticoids, including unreported metenolone acetate and dexamethasone 9,11-epoxide, were included in this method. Samples were dispersed in saturated sodium chloride containing 0.2% (v/v) acetic acid, and extracted with acetonitrile containing 0.2%(v/v) acetic acid. After that, an equal volume of water was added to the acetonitrile extraction solution to precipitate non-polar impurities. The solution was subsequently further purified using 10%(mass fraction) potassium ferrocyanide solution and 20%(mass fraction) zinc acetate solution containing 0.4% (v/v) acetic acid as precipitants. The sample solution was finally loaded onto a Waters ACQUITY UPLC BEH C₁₈ column (150 mm×3.0 mm, 1.7 μm) and gradient-eluted using aqueous and methanolic 0.2% (v/v) acetic acid solutions as mobile phases. The target compounds exhibited highly intense signals in positive electrospray-ionization mode. All compounds were analyzed in multiple reaction monitoring mode (MRM) and quantified using the external standard method. Rimexolone and hydrocortisone hemisuccinate hydrate exhibited peaks corresponding to their [M-H₂O+H]⁺ base ions, whereas the other 98 glucocorticoids exhibited [M+H]⁺ peaks. All positive samples were confirmed by their automated MRM-based information dependent acquisition (IDA) enhanced product ions (EPIs). Highly sensitive secondary mass spectra were acquired when EPI mode was combined with IDA and when target compounds in positive samples were located in MRM mode, with compounds further confirmed by matching their secondary mass spectra with those of the corresponding standard glycocorticoids using the Library Search function in SCIEX OS software.

Matrix effects (MEs) were investigated in water- and cream-based cosmetics by adding standard compounds to the extracted-matrix solutions. Ciclesonide exhibited no obvious matrix effect with a ME of 3.4% in the water-based matrix whereas it exhibited a serious inhibitory effect with a ME of 30.6% in the cream-based matrix. The remaining 99 target compounds exhibited MEs of -7.9%-12.4%, which are not significant because they are below 15%, further confirming that the sample-pretreatment method is effective and feasible. Therefore, ciclesonide in a cream-based matrix was quantified using a matrix-matched standard curve, while the others were quantified using solvent standard curves. The 100 glucocorticoids exhibited good linearities with correlation coefficients (r) of >0.99 in the range of 2.5-60 ng/mL. The limits of detection (LODs) and limits of quantification (LOQs) of this method were 0.03 and 0.1 μg/g, respectively. Recovery tests were performed at three spiked levels, namely one-, two-, and eight-times the LOQs. The 100 compounds exhibited recoveries of 79.6%-114.4% with relative standard deviations (RSDs) of 0.7%-9.4% (n=6) in water-based cosmetics; in comparison, they exhibited recoveries of 79.5%-112.1% with RSDs of 0.7%-12.9% (n=6) in cream-based cosmetics. Three cream-based positive samples were identified among 47 batches of cosmetics samples (including 25 batches of cream and lotion-based cosmetics, and 22 batches of water-based cosmetics), with quantitative analysis revealing five positive compounds: triamcinolone acetonide (115.1 μg/g), triamcinolone acetonide 21-acetate (0.6 μg/g), clobetasol propionate (24.5 μg/g), dexamethasone (2.7 μg/g), and dexamethasone-17-acetate (210.3 μg/g). These five compounds were further confirmed using MRM-IDA-EPI. The secondary mass spectra of the five compounds showed high matching degrees (>96%) with those of the corresponding standard glucocorticoids in the library database.

In conclusion, the method developed in this study is simple, practical, inexpensive, highly efficient, and suitable for qualitatively and quantitatively screening and analyzing 100 glucocorticoids in cosmetics, thereby filling supervisory gaps and greatly improving the detectability of glucocorticoids illegally added to cosmetics.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), glucocorticoid, cosmetic, illegally added

中图分类号:

O658

沈丹丹, 宫珊珊, 姜博海, 李悦忱, 薛恒跃, 于本涛, 柯亦梵, 李志远, 毛希琴. 超高效液相色谱-串联质谱法同时测定化妆品中100种糖皮质激素[J]. 色谱, 2024, 42(12): 1153-1163.

SHEN Dandan, GONG Shanshan, JIANG Bohai, LI Yuechen, XUE Hengyue, YU Bentao, KE Yifan, LI Zhiyuan, MAO Xiqin. Simultaneous determination of 100 glucocorticoids in cosmetics using ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2024, 42(12): 1153-1163.

图/表 4

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No.
1	deprodone (迪普罗酮)	20423-99-8	327.2	147.1^*/171.1	16.53	110	33/33
2	medrysone (甲羟松)	2668-66-8	345.2	327.3^*/135.2	24.09	100	20/27
3	methenolone acetate (美替诺龙醋酸酯)	434-05-9	345.3	187.2^*/303.4	26.77	125	30/25
4	cortexolone (脱氧可的松)	152-58-9	347.3	108.9^*/97.0	18.19	126	45/47
5	rimexolone (瑞美松龙)	49697-38-3	353.2	121.1^*/173.1	25.85	100	45/31
6	prednisone (泼尼松)	53-03-2	359.2	341.2^*/147.2	11.35	80	15/35
7	cortisone (可的松)	53-06-5	361.2	163.2^*/121.1	11.89	80	34/47
8	prednisolone (泼尼松龙)	50-24-8	361.2	343.2^*/147.2	13.71	80	14/34
9	hydrocortisone (氢化可的松)	50-23-7	363.2	121.1^*/105.0	13.68	80	31/68
10	meprednisone (甲基泼尼松)	1247-42-3	373.2	355.2^*/147.1	16.53	70	17/31
11	dexamethasone 9,11-epoxide (地塞米松9,11-环氧)	24916-90-3	373.1	355.3^*/337.3	17.79	90	17/16
12	methylprednisolone (甲基泼尼松龙)	83-43-2	375.2	357.1^*/161.1	18.02	66	14/28
13	16α-hydroxyprednisolone (16α-羟基泼尼松龙)	13951-70-7	377.2	359.2^*/147.1	9.41	70	17/30
14	6α-methyl hydrocortisone (6α-甲基氢化可的松)	1625-39-4	377.3	341.4^*/323.3	18.12	130	24/25
15	fluorometholone (氟米龙)	426-13-1	377.2	279.3^*/321.3	19.21	80	22/18
16	fluocortolone (氟可龙)	152-97-6	377.2	121.0^*/147.0	19.93	70	41/32
17	desoximetasone (去羟米松)	382-67-2	377.2	171.0^*/147.0	20.17	70	29/28
18	isoflupredone (异氟泼尼松)	338-95-4	379.3	359.2^*/341.2	12.39	90	14/18
19	fluprednisolone (氟泼尼龙)	53-34-9	379.1	341.3^*/323.2	12.68	95	16/17
20	fludrocortisone (氟氢可的松)	127-31-1	381.1	239.2^*/181.2	12.98	150	35/40
21	deflazacort (21-去乙酰基地夫可特)	13649-88-2	384.2	126.1^*/147.1	19.20	120	43/38
22	betamethasone base (倍他米松)	378-44-9	393.2	355.0^*/146.8	17.25	56	18/37
23	dexamethasone (地塞米松)	50-02-2	393.2	355.0^*/146.8	17.43	53	17/40
24	paramethasone (帕拉米松)	53-33-8	393.2	337.2^*/171.1	17.76	80	16/34
25	cloprednol (氯泼尼醇)	5251-34-3	393.2	205.0^*/271.1	20.11	80	32/25
26	triamcinolone (曲安西龙)	124-94-7	395.2	357.2^*/225.1	8.56	52	20/27
27	6α-fluoro-isoflupredone (6α-氟-异氟泼尼龙)	806-29-1	397.2	253.1^*/263.1	11.42	80	24/29
28	prednisone 21-acetate (泼尼松醋酸酯)	125-10-0	401.2	295.2^*/147.2	17.89	80	23/39
29	prednisolone-21-acetate (泼尼松龙醋酸酯)	52-21-1	403.3	307.2^*/367.3	18.20	85	20/15
30	cortisone acetate (可的松醋酸酯)	50-04-4	403.3	163.3^*/343.3	18.23	140	35/27
31	hydrocortisone acetate (氢化可的松醋酸酯)	50-03-3	405.3	309.2^*/120.8	18.17	80	25/24
32	beclomethasone (倍氯米松)	4419-39-0	409.2	147.1^*/279.1	18.15	106	39/41
33	diflorasone (双氟拉松)	2557-49-5	411.2	253.1^*/235.1	16.17	80	29/37
34	flumethasone (氟米松)	2135-17-3	411.3	253.2^*/121.0	16.43	80	22/50
35	clobetasol (氯倍他索)	25122-41-2	411.2	373.3^*/390.9	21.24	90	20/15
36	meprednisone acetate (甲泼尼松醋酸酯)	1106-03-2	415.1	327.2^*/147.1	21.01	120	22/34
37	desonide (地索奈德)	638-94-8	417.2	323.3^*/225.1	19.17	80	17/30
38	methylprednisolone acetate (甲基泼尼松龙醋酸酯)	53-36-1	417.2	253.2^*/399.2	21.49	80	28/28
39	16α-hydroxyprednisonlone acetate	86401-80-1	419.2	401.2^*/323.1	13.21	90	17/18
	(16α-羟基泼尼松龙醋酸酯)
40	eflone (氟米龙醋酸酯)	3801-06-7	419.3	279.2^*/321.2	21.72	80	20/19
41	isoflupredone acetate (异氟泼尼松醋酸酯)	338-98-7	421.2	401.3^*/383.3	17.24	90	13/16
42	fludrocortisone acetate (氟氢可的松醋酸酯)	514-36-3	423.4	239.2^*/343.2	17.79	170	35/30
43	mometasone (莫美他松)	105102-22-5	427.2	409.3^*/237.4	22.03	100	17/35
44	budesonide (布地奈德)	51333-22-3	431.2	413.2^*/147.1	23.73	40	15/33
45	hydrocortisone-17-butyrate (氢化可的松丁酸酯)	13609-67-1	433.3	345.0^*/120.8	22.96	80	22/23
46	triamcinolone acetonide (曲安奈德)	76-25-5	435.3	415.3^*/357.2	18.08	100	15/20
47	flunisolide (氟尼缩松)	3385-03-3	435.2	321.2^*/397.1	18.94	80	18/19
48	betamethasone 21-acetate (倍他米松醋酸酯)	987-24-6	435.3	337.0^*/309.0	20.77	80	15/15
49	dexamethasone-17-acetate (地塞米松醋酸酯)	1177-87-3	435.3	337.0^*/309.0	21.26	80	17/15
50	paramethasone acetate (帕拉米松醋酸酯)	1597-82-6	435.2	319.1^*/171.1	21.47	75	19/40
51	flurandrenolide (氟氢缩松)	1524-88-5	437.3	361.2^*/285.2	19.38	80	24/29
52	9-fluoro-16α,17-(isopropylidenedioxy)corticosterone (氢化曲安奈德)	1524-86-3	437.2	341.1^*/283.1	19.70	120	30/36
53	deflazacort (地夫可特)	14484-47-0	442.3	123.9^*/141.9	20.72	80	45/65
54	halometasone (卤美他松)	50629-82-8	445.2	154.8^*/287.0	18.61	80	45/34
55	prednisolone 21-trimethylacetate (泼尼松龙戊酸酯)	1107-99-9	445.3	427.2^*/307.2	24.94	90	18/25
56	cortisol 17-valerate (氢化可的松戊酸酯)	57524-89-7	447.3	345.3^*/121.1	24.50	80	19/39
57	betamethasone 17-propionate (倍他米松丙酸酯)	5534-13-4	449.2	355.2^*/279.2	22.93	90	16/24
58	fluocinolone acetonide (氟轻松)	67-73-2	453.2	337.1^*/121.0	18.30	80	21/46
59	flumethasone-17-acetate (双氟美松醋酸酯)	2823-42-9	453.1	253.2^*/335.3	20.34	110	25/20
60	halcinonide (哈西奈德)	3093-35-4	455.3	377.3^*/341.2	24.58	170	33/33
61	desonide 21-acetate (21-醋酸地索奈德)	25092-25-5	459.3	441.3^*/323.1	23.90	100	16/23
62	prednisolone tebutate (泼尼松龙丁醋酸酯)	7681-14-3	459.3	441.2^*/307.2	25.65	90	16/27
63	prednisolone succinate (泼尼松龙半琥珀酸酯)	2920-86-7	461.2	307.2^*/147.1	17.37	80	22/37
64	hydrocortisone (醋丙氢可的松)	74050-20-7	461.2	387.2^*/309.3	23.21	80	15/26
65	fluocortolone pivalate (氟可龙特戊酸酯)	29205-06-9	461.3	443.4^*/321.2	26.14	110	17/20
66	hydrocortisone hemisuccinate hydrate (氢化可的松琥珀酸酯)	83784-20-7	463.3	327.2^*/309.3	17.33	145	23/25
67	tixocortol pivalate (替可的松特戊酸酯)	55560-96-8	463.2	343.2^*/361.2	25.17	80	26/25
68	clobetasol propionate (氯倍他索丙酸酯)	25122-46-7	467.2	373.2^*/355.2	24.55	80	18/13
69	loteprednol (氯替泼诺)	82034-46-6	467.2	359.1^*/265.1	24.65	80	26/17
70	methylprednisolone aceponate (甲基泼尼松龙乙丙酸酯)	86401-95-8	473.3	455.2^*/381.2	24.40	90	16/17
71	methylprednisolone hemisuccinate (甲基泼尼松龙琥珀酸酯)	2921-57-5	475	457.0^*/339.0	20.67	80	14/17
72	triamcinolone acetonide 21-acetate (曲安奈德醋酸酯)	3870-07-3	477.2	339.2^*/321.2	23.31	80	22/23
73	dexamethasone valerate (地塞米松戊酸酯)	33755-46-3	477.3	355.2^*/279.2	24.61	90	16/26
74	betamethasone 17-valerate (倍他米松戊酸酯)	2152-44-5	477.2	355.3^*/279.3	25.23	80	18/24
75	dexamethasone 21-pivalate (地塞米松特戊酸酯)	1926-94-9	477.3	355.1^*/337.1	25.69	100	20/20
76	triamcinolone diacetate (曲安西龙双醋酸酯)	67-78-7	479.2	441.2^*/321.1	15.12	81	14/19
77	clobetasone butyrate (氯倍他松丁酸酯)	25122-57-0	479.3	343.2^*/279.2	25.36	86	24/24
78	diflucortolone valerate (双氟可龙戊酸酯)	59198-70-8	479.2	375.3^*/439.4	26.05	80	18/17
79	fluocinonide 22 methyl homologue (醋酸氟轻松22-甲基同系物)	51333-59-6	481.2	441.2^*/253.1	21.56/21.87	90	21/30
80	halobetasol propionate (卤倍他索丙酸酯)	66852-54-8	485.2	391.2^*/353.1	24.34	80	17/20
81	prednisolone valerate acetate (泼尼松龙醋酸戊酸酯)	72064-79-0	487.2	367.3^*/469.3	25.28	120	18/14
82	hydrocortisone cypionate (氢化可的松环戊丙酸酯)	508-99-6	487.6	327.3^*/309.3	26.74	170	27/29
83	prednicarbate (泼尼卡酯)	73771-04-7	489.2	381.3^*/115.1	24.77	80	16/25
84	hydrocortisone butyrate propionate (丙丁酸氢化可的松)	72590-77-3	489.4	401.4^*/327.3	25.48	120	20/30
85	diflorasone diacetate (二氟拉松双醋酸酯)	33564-31-7	495.3	317.1^*/307.3	23.09	110	20/25
86	fluocinonide (氟轻松醋酸酯)	356-12-7	495.3	455.4^*/319.3	23.30	120	20/22
87	flumethasone 21-pivalate (氟米松特戊酸酯)	2002-29-1	495.4	477.4^*/373.3	25.31	110	15/20
88	clocortolone pivalate (氯可托龙特戊酸酯)	34097-16-0	495.3	477.4^*/457.3	26.43	110	16/20
89	betamethasone benzoate (苯甲酸倍他米松)	22298-29-9	497.3	355.3^*/337.2	25.55	100	16/20
90	dexamethasone isonicotinate (地塞米松异烟酸酯)	2265-64-7	498.3	478.4^*/460.4	23.33	110	21/25
91	fluticasone propionate (氟替卡松丙酸酯)	80474-14-2	501.2	313.2^*/293.2	24.68	80	22/20
92	amcinonide (安西奈德)	51022-69-6	503.4	483.3^*/399.3	25.28	105	14/17
93	betamethasone 17,21-dipropionate (倍他米松双丙酸酯)	5593-20-4	505.3	319.2^*/279.1	25.51	71	20/35
94	difluprednate (双氟泼尼酯)	23674-86-4	509.2	303.3^*/279.3	23.66	110	22/22
95	betamethasone butyrate propionate (倍他米松丁酸丙酸酯)	5534-02-1	519.4	411.2^*/319.3	26.17	110	18/25
96	alclometasone dipropionate (阿氯米松双丙酸酯)	66734-13-2	521.4	503.3^*/319.2	24.38	105	13/20
97	mometasone furoate (莫米他松糠酸酯)	83919-23-7	521.3	503.2^*/355.2	24.63	100	17/24
98	beclomethasone dipropionate (倍氯米松双丙酸酯)	5534-09-8	521.1	503.2^*/319.2	25.95	80	16/23
99	triamcinolone hexacetonide (己曲安奈德)	5611-51-8	533.3	415.2^*/397.2	26.97	90	22/23
100	ciclesonide(环索奈德)	126544-47-6	541.4	523.4^*/305.3	28.49	115	18/28

No.
1	deprodone (迪普罗酮)	20423-99-8	327.2	147.1^*/171.1	16.53	110	33/33
2	medrysone (甲羟松)	2668-66-8	345.2	327.3^*/135.2	24.09	100	20/27
3	methenolone acetate (美替诺龙醋酸酯)	434-05-9	345.3	187.2^*/303.4	26.77	125	30/25
4	cortexolone (脱氧可的松)	152-58-9	347.3	108.9^*/97.0	18.19	126	45/47
5	rimexolone (瑞美松龙)	49697-38-3	353.2	121.1^*/173.1	25.85	100	45/31
6	prednisone (泼尼松)	53-03-2	359.2	341.2^*/147.2	11.35	80	15/35
7	cortisone (可的松)	53-06-5	361.2	163.2^*/121.1	11.89	80	34/47
8	prednisolone (泼尼松龙)	50-24-8	361.2	343.2^*/147.2	13.71	80	14/34
9	hydrocortisone (氢化可的松)	50-23-7	363.2	121.1^*/105.0	13.68	80	31/68
10	meprednisone (甲基泼尼松)	1247-42-3	373.2	355.2^*/147.1	16.53	70	17/31
11	dexamethasone 9,11-epoxide (地塞米松9,11-环氧)	24916-90-3	373.1	355.3^*/337.3	17.79	90	17/16
12	methylprednisolone (甲基泼尼松龙)	83-43-2	375.2	357.1^*/161.1	18.02	66	14/28
13	16α-hydroxyprednisolone (16α-羟基泼尼松龙)	13951-70-7	377.2	359.2^*/147.1	9.41	70	17/30
14	6α-methyl hydrocortisone (6α-甲基氢化可的松)	1625-39-4	377.3	341.4^*/323.3	18.12	130	24/25
15	fluorometholone (氟米龙)	426-13-1	377.2	279.3^*/321.3	19.21	80	22/18
16	fluocortolone (氟可龙)	152-97-6	377.2	121.0^*/147.0	19.93	70	41/32
17	desoximetasone (去羟米松)	382-67-2	377.2	171.0^*/147.0	20.17	70	29/28
18	isoflupredone (异氟泼尼松)	338-95-4	379.3	359.2^*/341.2	12.39	90	14/18
19	fluprednisolone (氟泼尼龙)	53-34-9	379.1	341.3^*/323.2	12.68	95	16/17
20	fludrocortisone (氟氢可的松)	127-31-1	381.1	239.2^*/181.2	12.98	150	35/40
21	deflazacort (21-去乙酰基地夫可特)	13649-88-2	384.2	126.1^*/147.1	19.20	120	43/38
22	betamethasone base (倍他米松)	378-44-9	393.2	355.0^*/146.8	17.25	56	18/37
23	dexamethasone (地塞米松)	50-02-2	393.2	355.0^*/146.8	17.43	53	17/40
24	paramethasone (帕拉米松)	53-33-8	393.2	337.2^*/171.1	17.76	80	16/34
25	cloprednol (氯泼尼醇)	5251-34-3	393.2	205.0^*/271.1	20.11	80	32/25
26	triamcinolone (曲安西龙)	124-94-7	395.2	357.2^*/225.1	8.56	52	20/27
27	6α-fluoro-isoflupredone (6α-氟-异氟泼尼龙)	806-29-1	397.2	253.1^*/263.1	11.42	80	24/29
28	prednisone 21-acetate (泼尼松醋酸酯)	125-10-0	401.2	295.2^*/147.2	17.89	80	23/39
29	prednisolone-21-acetate (泼尼松龙醋酸酯)	52-21-1	403.3	307.2^*/367.3	18.20	85	20/15
30	cortisone acetate (可的松醋酸酯)	50-04-4	403.3	163.3^*/343.3	18.23	140	35/27
31	hydrocortisone acetate (氢化可的松醋酸酯)	50-03-3	405.3	309.2^*/120.8	18.17	80	25/24
32	beclomethasone (倍氯米松)	4419-39-0	409.2	147.1^*/279.1	18.15	106	39/41
33	diflorasone (双氟拉松)	2557-49-5	411.2	253.1^*/235.1	16.17	80	29/37
34	flumethasone (氟米松)	2135-17-3	411.3	253.2^*/121.0	16.43	80	22/50
35	clobetasol (氯倍他索)	25122-41-2	411.2	373.3^*/390.9	21.24	90	20/15
36	meprednisone acetate (甲泼尼松醋酸酯)	1106-03-2	415.1	327.2^*/147.1	21.01	120	22/34
37	desonide (地索奈德)	638-94-8	417.2	323.3^*/225.1	19.17	80	17/30
38	methylprednisolone acetate (甲基泼尼松龙醋酸酯)	53-36-1	417.2	253.2^*/399.2	21.49	80	28/28
39	16α-hydroxyprednisonlone acetate	86401-80-1	419.2	401.2^*/323.1	13.21	90	17/18
	(16α-羟基泼尼松龙醋酸酯)
40	eflone (氟米龙醋酸酯)	3801-06-7	419.3	279.2^*/321.2	21.72	80	20/19
41	isoflupredone acetate (异氟泼尼松醋酸酯)	338-98-7	421.2	401.3^*/383.3	17.24	90	13/16
42	fludrocortisone acetate (氟氢可的松醋酸酯)	514-36-3	423.4	239.2^*/343.2	17.79	170	35/30
43	mometasone (莫美他松)	105102-22-5	427.2	409.3^*/237.4	22.03	100	17/35
44	budesonide (布地奈德)	51333-22-3	431.2	413.2^*/147.1	23.73	40	15/33
45	hydrocortisone-17-butyrate (氢化可的松丁酸酯)	13609-67-1	433.3	345.0^*/120.8	22.96	80	22/23
46	triamcinolone acetonide (曲安奈德)	76-25-5	435.3	415.3^*/357.2	18.08	100	15/20
47	flunisolide (氟尼缩松)	3385-03-3	435.2	321.2^*/397.1	18.94	80	18/19
48	betamethasone 21-acetate (倍他米松醋酸酯)	987-24-6	435.3	337.0^*/309.0	20.77	80	15/15
49	dexamethasone-17-acetate (地塞米松醋酸酯)	1177-87-3	435.3	337.0^*/309.0	21.26	80	17/15
50	paramethasone acetate (帕拉米松醋酸酯)	1597-82-6	435.2	319.1^*/171.1	21.47	75	19/40
51	flurandrenolide (氟氢缩松)	1524-88-5	437.3	361.2^*/285.2	19.38	80	24/29
52	9-fluoro-16α,17-(isopropylidenedioxy)corticosterone (氢化曲安奈德)	1524-86-3	437.2	341.1^*/283.1	19.70	120	30/36
53	deflazacort (地夫可特)	14484-47-0	442.3	123.9^*/141.9	20.72	80	45/65
54	halometasone (卤美他松)	50629-82-8	445.2	154.8^*/287.0	18.61	80	45/34
55	prednisolone 21-trimethylacetate (泼尼松龙戊酸酯)	1107-99-9	445.3	427.2^*/307.2	24.94	90	18/25
56	cortisol 17-valerate (氢化可的松戊酸酯)	57524-89-7	447.3	345.3^*/121.1	24.50	80	19/39
57	betamethasone 17-propionate (倍他米松丙酸酯)	5534-13-4	449.2	355.2^*/279.2	22.93	90	16/24
58	fluocinolone acetonide (氟轻松)	67-73-2	453.2	337.1^*/121.0	18.30	80	21/46
59	flumethasone-17-acetate (双氟美松醋酸酯)	2823-42-9	453.1	253.2^*/335.3	20.34	110	25/20
60	halcinonide (哈西奈德)	3093-35-4	455.3	377.3^*/341.2	24.58	170	33/33
61	desonide 21-acetate (21-醋酸地索奈德)	25092-25-5	459.3	441.3^*/323.1	23.90	100	16/23
62	prednisolone tebutate (泼尼松龙丁醋酸酯)	7681-14-3	459.3	441.2^*/307.2	25.65	90	16/27
63	prednisolone succinate (泼尼松龙半琥珀酸酯)	2920-86-7	461.2	307.2^*/147.1	17.37	80	22/37
64	hydrocortisone (醋丙氢可的松)	74050-20-7	461.2	387.2^*/309.3	23.21	80	15/26
65	fluocortolone pivalate (氟可龙特戊酸酯)	29205-06-9	461.3	443.4^*/321.2	26.14	110	17/20
66	hydrocortisone hemisuccinate hydrate (氢化可的松琥珀酸酯)	83784-20-7	463.3	327.2^*/309.3	17.33	145	23/25
67	tixocortol pivalate (替可的松特戊酸酯)	55560-96-8	463.2	343.2^*/361.2	25.17	80	26/25
68	clobetasol propionate (氯倍他索丙酸酯)	25122-46-7	467.2	373.2^*/355.2	24.55	80	18/13
69	loteprednol (氯替泼诺)	82034-46-6	467.2	359.1^*/265.1	24.65	80	26/17
70	methylprednisolone aceponate (甲基泼尼松龙乙丙酸酯)	86401-95-8	473.3	455.2^*/381.2	24.40	90	16/17
71	methylprednisolone hemisuccinate (甲基泼尼松龙琥珀酸酯)	2921-57-5	475	457.0^*/339.0	20.67	80	14/17
72	triamcinolone acetonide 21-acetate (曲安奈德醋酸酯)	3870-07-3	477.2	339.2^*/321.2	23.31	80	22/23
73	dexamethasone valerate (地塞米松戊酸酯)	33755-46-3	477.3	355.2^*/279.2	24.61	90	16/26
74	betamethasone 17-valerate (倍他米松戊酸酯)	2152-44-5	477.2	355.3^*/279.3	25.23	80	18/24
75	dexamethasone 21-pivalate (地塞米松特戊酸酯)	1926-94-9	477.3	355.1^*/337.1	25.69	100	20/20
76	triamcinolone diacetate (曲安西龙双醋酸酯)	67-78-7	479.2	441.2^*/321.1	15.12	81	14/19
77	clobetasone butyrate (氯倍他松丁酸酯)	25122-57-0	479.3	343.2^*/279.2	25.36	86	24/24
78	diflucortolone valerate (双氟可龙戊酸酯)	59198-70-8	479.2	375.3^*/439.4	26.05	80	18/17
79	fluocinonide 22 methyl homologue (醋酸氟轻松22-甲基同系物)	51333-59-6	481.2	441.2^*/253.1	21.56/21.87	90	21/30
80	halobetasol propionate (卤倍他索丙酸酯)	66852-54-8	485.2	391.2^*/353.1	24.34	80	17/20
81	prednisolone valerate acetate (泼尼松龙醋酸戊酸酯)	72064-79-0	487.2	367.3^*/469.3	25.28	120	18/14
82	hydrocortisone cypionate (氢化可的松环戊丙酸酯)	508-99-6	487.6	327.3^*/309.3	26.74	170	27/29
83	prednicarbate (泼尼卡酯)	73771-04-7	489.2	381.3^*/115.1	24.77	80	16/25
84	hydrocortisone butyrate propionate (丙丁酸氢化可的松)	72590-77-3	489.4	401.4^*/327.3	25.48	120	20/30
85	diflorasone diacetate (二氟拉松双醋酸酯)	33564-31-7	495.3	317.1^*/307.3	23.09	110	20/25
86	fluocinonide (氟轻松醋酸酯)	356-12-7	495.3	455.4^*/319.3	23.30	120	20/22
87	flumethasone 21-pivalate (氟米松特戊酸酯)	2002-29-1	495.4	477.4^*/373.3	25.31	110	15/20
88	clocortolone pivalate (氯可托龙特戊酸酯)	34097-16-0	495.3	477.4^*/457.3	26.43	110	16/20
89	betamethasone benzoate (苯甲酸倍他米松)	22298-29-9	497.3	355.3^*/337.2	25.55	100	16/20
90	dexamethasone isonicotinate (地塞米松异烟酸酯)	2265-64-7	498.3	478.4^*/460.4	23.33	110	21/25
91	fluticasone propionate (氟替卡松丙酸酯)	80474-14-2	501.2	313.2^*/293.2	24.68	80	22/20
92	amcinonide (安西奈德)	51022-69-6	503.4	483.3^*/399.3	25.28	105	14/17
93	betamethasone 17,21-dipropionate (倍他米松双丙酸酯)	5593-20-4	505.3	319.2^*/279.1	25.51	71	20/35
94	difluprednate (双氟泼尼酯)	23674-86-4	509.2	303.3^*/279.3	23.66	110	22/22
95	betamethasone butyrate propionate (倍他米松丁酸丙酸酯)	5534-02-1	519.4	411.2^*/319.3	26.17	110	18/25
96	alclometasone dipropionate (阿氯米松双丙酸酯)	66734-13-2	521.4	503.3^*/319.2	24.38	105	13/20
97	mometasone furoate (莫米他松糠酸酯)	83919-23-7	521.3	503.2^*/355.2	24.63	100	17/24
98	beclomethasone dipropionate (倍氯米松双丙酸酯)	5534-09-8	521.1	503.2^*/319.2	25.95	80	16/23
99	triamcinolone hexacetonide (己曲安奈德)	5611-51-8	533.3	415.2^*/397.2	26.97	90	22/23
100	ciclesonide(环索奈德)	126544-47-6	541.4	523.4^*/305.3	28.49	115	18/28

Compound No.	Linear equation	r	Water-based (n=6)		Cream-based (n=6)
Compound No.	Linear equation	r	Recoveries^*/%	RSDs^*/%	Recoveries^*/%	RSDs^*/%
1	y=1.12×10⁴x+2.65×10³	0.9984	88.6, 111.7, 103.5	5.6, 2.8, 2.5	90.9, 100.6, 94.5	5.5, 6.4, 5.7
2	y=5.40×10⁴x+2.03×10³	0.9994	86.3, 108.0, 94.4	5.7, 3.6, 2.8	98.9, 105.7, 102.2	2.8, 3.0, 1.5
3	y=7.26×10⁴x+5.57×10³	0.9998	86.5, 105.6, 99.2	6.1, 3.1, 3.0	91.4, 98.4, 94.4	3.3, 3.1, 1.5
4	y=3.58×10⁴x+2.13×10⁴	0.9965	87.1, 109.7, 104.3	4.8, 2.3, 2.0	89.6, 107.5, 105.6	4.7, 2.9, 2.2
5	y=9.95×10³x+6.46×10²	0.9977	84.8, 106.7, 94.7	6.3, 4.6, 2.9	99.3, 101.1, 99.5	8.3, 6.7, 2.6
6	y=4.29×10⁴x+2.14×10³	0.9994	97.9, 106.4, 106.2	5.2, 2.9, 1.5	93.0, 98.1, 105.6	3.2, 1.8, 3.4
7	y=4.83×10⁴x+1.07×10²	0.9994	92.3, 105.5, 103.5	5.3, 3.2, 1.8	88.5, 99.6, 98.4	3.8, 3.5, 2.4
8	y=8.82×10⁴x+8.19×10³	0.9989	93.0, 106.4, 102.7	6.8, 2.5, 1.7	86.0, 99.8, 99.9	4.1, 4.1, 2.8
9	y=2.34×10⁴x+2.37×10³	0.9985	91.7, 106.3, 102.6	7.2, 3.4, 2.3	84.5, 101.6, 100.1	3.9, 3.8, 2.9
10	y=5.35×10⁴x+7.73×10³	0.9992	93.9, 111.0, 102.1	5.8, 2.4, 2.6	84.6, 103.2, 93.0	9.2, 3.2, 7.1
11	y=3.79×10⁴x+1.27×10⁴	0.9981	92.7, 112.8, 105.9	4.3, 1.5, 1.4	87.3, 105.5, 107.4	7.2, 3.9, 1.4
12	y=8.62×10⁴x+3.55×10³	0.9985	94.4, 106.6, 102.5	7.8, 3.6, 2.2	96.0, 104.7, 105.2	6.0, 3.3, 2.1
13	y=7.41×10⁴x+0.96×10²	0.9996	94.9, 94.0, 97.7	5.8, 3.5, 1.9	86.2, 79.5, 91.7	2.9, 6.2, 1.8
14	y=1.52×10⁴x+1.00×10⁴	0.9970	82.7, 103.8, 102.0	8.5, 4.0, 3.0	91.1, 107.5, 107.4	9.3, 3.9, 3.8
15	y=4.95×10⁴x+1.68×10⁴	0.9981	87.1, 112.7, 100.0	5.5, 1.6, 1.2	94.6, 110.3, 104.8	2.0, 2.3, 1.7
16	y=1.23×10⁴x+1.19×10²	0.9998	92.9, 108.6, 102.4	6.2, 1.9, 2.3	95.4, 105.9, 103.0	4.4, 2.4, 2.0
17	y=1.82×10⁴x+7.94×10²	0.9998	91.8, 103.9, 101.3	6.1, 2.6, 2.1	98.2, 102.5, 104.5	2.4, 1.9, 1.1
18	y=6.87×10⁴x-2.60×10³	0.9997	100.5, 104.4, 107.3	4.6, 1.9, 1.8	94.3, 98.2, 105.4	3.2, 3.1, 2.3
19	y=1.90×10⁴x-1.99×10³	0.9996	96.9, 105.5, 107.2	5.6, 3.1, 2.4	93.4, 99.0, 106.1	3.6, 1.7, 2.6
20	y=1.39×10⁴x-1.47×10³	0.9999	99.2, 100.1, 106.8	6.4, 3.4, 1.5	93.8, 91.5, 106.2	3.7, 3.1, 2.6
21	y=4.39×10⁴x+1.26×10⁴	0.9984	84.8, 107.6, 95.0	4.3, 0.9, 2.8	101.3, 103.4, 101.6	3.0, 2.6, 1.9
22	y=3.35×10⁴x+8.91×10³	0.9975	92.1, 107.1, 105.4	6.0, 4.0, 2.5	97.6, 102.6, 105.2	7.1, 3.8, 1.6
23	y=7.12×10⁴x+1.64×10⁴	0.9978	91.7, 109.1, 103.9	6.1, 3.7, 2.3	93.1, 105.8, 104.9	6.6, 3.9, 2.0
24	y=4.38×10⁴x+7.62×10³	0.9984	98.4, 109.4, 107.0	6.3, 4.2, 2.5	96.8, 102.1, 107.8	5.8, 2.2, 2.4
25	y=9.84×10³x-1.97×10³	0.9994	94.0, 107.3, 98.8	4.4, 3.7, 2.2	91.8, 102.6, 101.3	5.1, 2.8, 1.2
26	y=4.27×10⁴x-4.32×10³	0.9995	93.5, 96.6, 99.8	5.2, 1.8, 1.8	90.7, 88.9, 101.5	3.3, 2.8, 1.4
27	y=2.92×10⁴x+1.44×10³	0.9991	96.9, 106.6, 105.6	5.3, 2.0, 1.9	94.5, 100.7, 107.1	4.1, 2.7, 2.2
28	y=3.47×10⁴x+2.50×10³	0.9990	86.9, 108.2, 97.5	4.3, 2.1, 2.1	93.7, 102.1, 100.1	4.7, 2.8, 2.4
29	y=2.66×10⁴x+1.27×10⁴	0.9971	85.9, 107.6, 100.8	6.0, 3.8, 1.7	93.8, 108.0, 103.4	4.4, 2.7, 1.9
30	y=4.07×10⁴x+1.63×10⁴	0.9980	83.1, 108.2, 98.2	5.1, 2.2, 2.1	92.3, 104.0, 103.0	4.8, 2.6, 2.1
31	y=2.64×10⁴x+1.73×10⁴	0.9937	80.5, 110.9, 100.0	7.6, 3.4, 1.8	91.9, 109.2, 104.0	3.6, 2.4, 1.7
32	y=7.75×10³x+4.87×10³	0.9928	94.8, 98.0, 103.5	7.2, 4.9, 0.7	88.7, 109.3, 106.6	6.5, 2.6, 1.7
33	y=1.28×10⁴x-7.76×10²	0.9996	92.6, 103.3, 102.0	4.2, 2.4, 2.6	95.0, 104.2, 103.5	2.2, 2.1, 3.4
34	y=3.62×10⁴x+2.58×10³	0.9992	94.2, 107.7, 101.5	6.1, 2.4, 3.5	84.1, 102.6, 92.8	12.0, 2.9, 12.9
35	y=5.73×10⁴x+9.50×10³	0.9983	86.4, 109.6, 99.5	5.0, 2.2, 1.7	96.8, 107.2, 104.0	3.6, 2.3, 2.1
36	y=1.88×10⁴x-9.66×10²	0.9997	85.9, 105.4, 92.1	6.2, 4.0, 2.4	88.2, 105.3, 100.8	5.1, 3.6, 2.2
37	y=4.73×10⁴x+1.13×10⁴	0.9966	94.4, 111.1, 105.0	6.7, 2.2, 1.7	91.3, 103.9, 104.3	2.7, 1.4, 1.8
38	y=1.93×10⁴x+6.83×10²	0.9989	87.5, 106.0, 98.2	5.5, 1.7, 2.8	104.5, 104.5, 105.5	5.7, 2.6, 1.8
39	y=6.78×10⁴x-2.80×10³	0.9998	92.3, 102.0, 100.9	4.7, 1.9, 2.3	98.1, 98.3, 104.7	3.1, 2.5, 2.1
40	y=1.18×10⁵x+1.10×10⁴	0.9990	87.4, 109.8, 98.2	6.3, 2.1, 1.6	98.2, 105.1, 102.4	3.5, 1.6, 2.1
41	y=5.26×10⁴x+1.30×10⁴	0.9988	85.0, 109.6, 97.8	5.2, 2.2, 1.8	99.0, 106.8, 102.6	3.6, 2.1, 2.4
42	y=1.02×10⁴x+4.03×10³	0.9957	84.1, 109.4, 98.0	8.5, 3.9, 1.6	105.8, 101.9, 103.4	7.4, 6.0, 1.8
43	y=5.53×10⁴x+7.11×10³	0.9993	85.9, 107.5, 97.1	5.6, 2.4, 1.5	97.4, 108.7, 103.4	2.2, 2.8, 2.1
44	y=8.67×10⁴x+1.17×10³	0.9995	86.1, 107.0, 93.6	5.8, 2.2, 2.1	96.9, 107.0, 100.5	4.3, 2.9, 2.4
45	y=4.99×10⁴x+1.40×10⁴	0.9988	86.7, 105.1, 99.0	5.6, 2.8, 2.2	96.5, 106.9, 105.3	4.0, 3.3, 1.8
46	y=6.95×10⁴x+1.41×10⁴	0.9967	87.9, 102.9, 98.9	5.4, 2.8, 2.0	94.6, 105.0, 107.3	3.4, 3.6, 1.7
47	y=4.45×10⁴x-2.78×10³	0.9993	94.3, 108.6, 102.7	5.9, 2.4, 2.4	94.0, 102.4, 102.5	2.5, 1.2, 1.7
48	y=8.99×10³x+9.66×10²	0.9996	83.6, 109.1, 96.8	6.4, 4.0, 1.8	95.5, 104.2, 102.8	5.7, 3.4, 1.4
49	y=1.75×10⁴x+1.81×10³	0.9992	86.8, 105.9, 96.7	6.2, 2.3, 1.2	99.0, 105.8, 103.8	3.2, 5.6, 1.4
50	y=2.31×10⁴x+3.25×10³	0.9996	87.1, 106.5, 98.7	6.6, 1.5, 1.4	98.3, 107.0, 104.3	5.1, 3.0, 1.3
51	y=1.68×10⁴x-1.52×10³	0.9997	97.5, 106.8, 103.1	6.9, 3.7, 2.4	91.1, 102.3, 102.3	2.1, 2.8, 2.0
52	y=1.07×10⁴x+1.17×10³	0.9997	82.1, 104.0, 97.7	8.6, 1.7, 1.5	100.1, 98.4, 100.8	3.5, 4.3, 2.4
53	y=1.09×10⁴x-2.33×10²	0.9985	86.6, 105.3, 93.3	6.0, 2.2, 2.6	102.1, 104.6, 101.9	3.5, 3.4, 2.3
54	y=1.13×10⁴x+8.04×10²	0.9997	88.7, 105.2, 102.6	6.3, 2.6, 1.6	98.0, 99.1, 104.4	4.2, 4.0, 2.5
55	y=1.07×10⁵x-1.45×10³	0.9991	84.7, 107.1, 93.8	6.4, 1.5, 2.8	94.9, 107.8, 94.4	4.8, 2.3, 2.4
56	y=6.49×10⁴x+4.88×10³	0.9993	88.6, 107.6, 98.4	5.8, 3.6, 1.6	100.9, 101.2, 103.6	2.6, 3.3, 1.0
57	y=1.56×10⁵x+4.83×10⁴	0.9972	87.0, 109.7, 99.0	6.1, 2.2, 2.0	96.6, 108.1, 104.8	3.4, 1.4, 1.5
58	y=3.00×10⁴x+3.92×10³	0.9985	90.2, 108.4, 102.2	5.3, 2.6, 2.1	96.6, 103.3, 104.8	4.8, 4.3, 2.7
59	y=1.62×10⁴x-3.42×10²	0.9999	86.1, 105.6, 95.5	5.7, 2.6, 1.5	93.2, 105.8, 102.6	5.3, 1.8, 2.0
60	y=8.93×10³x+1.77×10³	0.9980	84.3, 108.4, 97.3	6.6, 4.8, 1.3	88.1, 108.2, 103.5	7.3, 4.4, 1.5
61	y=1.29×10⁵x+1.79×10⁴	0.9990	81.0, 104.6, 93.2	5.0, 2.7, 2.0	91.4, 106.8, 96.6	4.5, 1.4, 4.1
62	y=1.09×10⁵x-1.83×10³	0.9996	85.9, 109.2, 94.9	5.9, 3.6, 2.0	99.5, 106.8, 100.6	3.2, 3.0, 1.5
63	y=2.12×10⁴x-2.68×10²	0.9993	99.5, 110.5, 105.4	6.6, 2.3, 1.7	95.9, 108.7, 104.5	7.4, 3.1, 0.9
64	y=3.88×10⁴x+2.89×10³	0.9996	85.0, 106.9, 95.8	5.9, 2.9, 2.5	98.0, 103.8, 99.0	3.2, 3.5, 1.2
65	y=3.23×10⁴x-0.37×10²	0.9993	84.7, 107.8, 95.1	5.0, 2.2, 2.7	91.7, 101.2, 98.8	5.2, 2.3, 1.2
66	y=2.73×10⁴x+3.01×10³	0.9990	97.5, 108.6, 107.2	7.6, 2.3, 1.8	94.7, 106.6, 105.0	2.7, 2.6, 1.8
67	y=1.79×10⁴x-1.80×10³	0.9992	82.6, 107.4, 91.4	8.8, 3.0, 1.7	97.5, 104.5, 101.9	6.1, 3.4, 3.2
68	y=4.98×10⁴x+1.08×10⁴	0.9992	82.7, 108.8, 97.0	8.6, 2.9, 1.4	97.0, 104.0, 104.1	3.8, 3.6, 2.8
69	y=5.12×10⁴x+9.36×10³	0.9984	85.4, 110.6, 98.1	8.4, 4.0, 3.0	98.0, 111.4, 105.2	7.2, 3.0, 1.4
70	y=9.26×10⁴x+2.56×10⁴	0.9983	79.7, 106.4, 94.3	7.2, 2.5, 1.2	98.1, 106.2, 102.4	5.8, 3.8, 2.2
71	y=2.87×10⁴x-3.48×10³	0.9998	91.7, 104.4, 99.3	6.2, 3.1, 2.2	100.3, 107.3, 102.7	6.3, 4.5, 1.0
72	y=4.68×10⁴x+8.92×10³	0.9981	86.6, 108.3, 98.5	4.7, 2.6, 1.9	96.1, 107.7, 100.1	2.8, 3.5, 1.5
73	y=4.24×10⁴x+5.47×10³	0.9979	89.1, 111.5, 98.6	6.1, 0.9, 2.5	97.1, 108.5, 104.0	2.7, 2.6, 1.6
74	y=8.01×10⁴x-3.76×10²	0.9995	88.9, 106.7, 96.7	6.0, 1.5, 1.5	98.0, 106.2, 100.3	3.2, 1.6, 1.1
75	y=5.82×10⁴x+4.28×10³	0.9995	80.3, 105.9, 92.9	6.3, 4.9, 1.3	96.0, 107.2, 97.8	4.3, 1.9, 1.8
76	y=5.12×10⁴x+4.08×10³	0.9990	86.8, 106.8, 98.1	5.5, 2.0, 1.2	98.3, 101.9, 102.8	4.3, 2.7, 2.2
77	y=3.08×10⁴x-3.61×10²	0.9987	86.7, 105.8, 94.9	5.7, 2.3, 2.5	104.4, 106.1, 99.5	5.0, 3.9, 2.7
78	y=3.49×10⁴x-2.10×10³	0.9995	84.5, 109.1, 95.2	6.3, 1.3, 2.1	102.0, 105.6, 99.5	6.0, 2.8, 1.6
79	y=2.68×10⁵x+1.67×10³	0.9993	87.6, 107.3, 97.7	6.2, 3.5, 2.4	96.9, 104.3, 101.8	4.2, 2.7, 1.7
80	y=2.15×10⁴x+2.52×10³	0.9995	81.1, 108.7, 91.9	6.4, 4.5, 1.5	96.6, 106.0, 97.7	3.6, 1.9, 2.3
81	y=6.34×10⁴x+2.53×10⁴	0.9972	79.9, 110.3, 96.8	7.5, 2.0, 2.1	95.8, 110.0, 99.1	5.3, 3.2, 2.1
82	y=1.83×10⁴x-2.41×10²	0.9995	83.1, 107.1, 95.5	7.1, 1.9, 2.7	95.3, 102.2, 93.9	4.4, 5.7, 1.3
83	y=8.21×10⁴x+2.05×10³	0.9989	83.2, 103.8, 92.7	6.0, 5.6, 1.4	93.8, 102.7, 98.8	5.6, 3.7, 1.5
84	y=6.38×10⁴x-4.05×10²	0.9993	86.2, 108.9, 96.4	6.3, 4.8, 3.5	98.7, 106.5, 99.3	4.4, 3.1, 1.7
85	y=2.97×10⁴x+4.26×10³	0.9992	83.6, 107.8, 96.0	6.5, 2.8, 2.2	98.4, 107.6, 102.3	4.6, 2.1, 1.5
86	y=1.58×10⁴x+4.51×10³	0.9980	87.5, 113.8, 99.0	5.8, 1.3, 1.0	92.1, 112.1, 101.0	3.1, 3.4, 3.1
87	y=1.45×10⁴x+6.08×10³	0.9982	80.0, 112.0, 97.9	9.4, 2.7, 2.2	93.7, 107.1, 105.9	5.6, 5.1, 1.7
88	y=3.36×10⁴x-0.79×10²	0.9996	83.9, 107.1, 94.7	7.4, 3.8, 1.9	104.2, 109.5, 99.3	3.8, 3.0, 3.2
89	y=7.14×10⁴x+2.47×10²	0.9988	90.0, 108.8, 96.4	5.4, 2.7, 1.7	99.0, 107.0, 101.9	6.6, 2.5, 0.7
90	y=6.94×10⁴x+1.85×10⁴	0.9983	83.6, 101.6, 95.6	7.3, 1.7, 2.1	84.9, 94.3, 94.6	5.1, 2.4, 2.4
91	y=4.77×10⁴x+6.96×10³	0.9988	84.9, 109.2, 96.7	7.2, 1.6, 1.8	97.4, 106.8, 103.6	4.4, 3.3, 1.2
92	y=6.10×10⁴x+2.75×10⁴	0.9955	81.3, 114.4, 98.3	8.4, 2.7, 2.3	97.6, 111.7, 103.4	5.1, 3.2, 1.2
93	y=2.81×10⁴x+3.21×10³	0.9993	81.3, 107.2, 96.7	7.8, 5.4, 1.9	98.1, 104.7, 98.5	2.6, 2.2, 0.9
94	y=3.83×10⁴x+8.97×10³	0.9989	81.1, 100.2, 95.2	5.1, 0.9, 2.2	100.0, 107.9, 102.8	2.5, 2.0, 1.9
95	y=7.20×10⁴x+1.10×10⁴	0.9994	81.1, 105.3, 97.1	6.3, 2.1, 2.8	97.1, 105.2, 99.6	5.3, 2.0, 1.6
96	y=1.95×10⁴x+5.24×10³	0.9984	79.6, 106.1, 93.7	8.4, 2.4, 2.0	94.3, 107.9, 103.2	7.2, 3.3, 1.2
97	y=4.78×10⁴x+1.76×10⁴	0.9970	79.7, 110.4, 96.5	8.5, 3.4, 1.7	96.0, 111.6, 102.6	1.5, 0.9, 1.2
98	y=8.82×10⁴x+9.81×10³	0.9989	82.5, 105.4, 96.3	7.8, 2.1, 2.2	97.6, 105.2, 99.6	4.1, 2.3, 2.1
99	y=1.15×10⁵x+9.19×10³	0.9996	82.5, 108.6, 94.7	6.5, 2.9, 1.8	94.6, 105.0, 96.9	3.2, 1.7, 0.9
100	y=1.65×10⁵x+3.65×10⁴	0.9998	81.6, 105.9, 98.4	9.2, 2.2, 3.6	88.1, 100.0, 80.9	2.5, 1.2, 1.3

Compound No.	Linear equation	r	Water-based (n=6)		Cream-based (n=6)
Compound No.	Linear equation	r	Recoveries^*/%	RSDs^*/%	Recoveries^*/%	RSDs^*/%
1	y=1.12×10⁴x+2.65×10³	0.9984	88.6, 111.7, 103.5	5.6, 2.8, 2.5	90.9, 100.6, 94.5	5.5, 6.4, 5.7
2	y=5.40×10⁴x+2.03×10³	0.9994	86.3, 108.0, 94.4	5.7, 3.6, 2.8	98.9, 105.7, 102.2	2.8, 3.0, 1.5
3	y=7.26×10⁴x+5.57×10³	0.9998	86.5, 105.6, 99.2	6.1, 3.1, 3.0	91.4, 98.4, 94.4	3.3, 3.1, 1.5
4	y=3.58×10⁴x+2.13×10⁴	0.9965	87.1, 109.7, 104.3	4.8, 2.3, 2.0	89.6, 107.5, 105.6	4.7, 2.9, 2.2
5	y=9.95×10³x+6.46×10²	0.9977	84.8, 106.7, 94.7	6.3, 4.6, 2.9	99.3, 101.1, 99.5	8.3, 6.7, 2.6
6	y=4.29×10⁴x+2.14×10³	0.9994	97.9, 106.4, 106.2	5.2, 2.9, 1.5	93.0, 98.1, 105.6	3.2, 1.8, 3.4
7	y=4.83×10⁴x+1.07×10²	0.9994	92.3, 105.5, 103.5	5.3, 3.2, 1.8	88.5, 99.6, 98.4	3.8, 3.5, 2.4
8	y=8.82×10⁴x+8.19×10³	0.9989	93.0, 106.4, 102.7	6.8, 2.5, 1.7	86.0, 99.8, 99.9	4.1, 4.1, 2.8
9	y=2.34×10⁴x+2.37×10³	0.9985	91.7, 106.3, 102.6	7.2, 3.4, 2.3	84.5, 101.6, 100.1	3.9, 3.8, 2.9
10	y=5.35×10⁴x+7.73×10³	0.9992	93.9, 111.0, 102.1	5.8, 2.4, 2.6	84.6, 103.2, 93.0	9.2, 3.2, 7.1
11	y=3.79×10⁴x+1.27×10⁴	0.9981	92.7, 112.8, 105.9	4.3, 1.5, 1.4	87.3, 105.5, 107.4	7.2, 3.9, 1.4
12	y=8.62×10⁴x+3.55×10³	0.9985	94.4, 106.6, 102.5	7.8, 3.6, 2.2	96.0, 104.7, 105.2	6.0, 3.3, 2.1
13	y=7.41×10⁴x+0.96×10²	0.9996	94.9, 94.0, 97.7	5.8, 3.5, 1.9	86.2, 79.5, 91.7	2.9, 6.2, 1.8
14	y=1.52×10⁴x+1.00×10⁴	0.9970	82.7, 103.8, 102.0	8.5, 4.0, 3.0	91.1, 107.5, 107.4	9.3, 3.9, 3.8
15	y=4.95×10⁴x+1.68×10⁴	0.9981	87.1, 112.7, 100.0	5.5, 1.6, 1.2	94.6, 110.3, 104.8	2.0, 2.3, 1.7
16	y=1.23×10⁴x+1.19×10²	0.9998	92.9, 108.6, 102.4	6.2, 1.9, 2.3	95.4, 105.9, 103.0	4.4, 2.4, 2.0
17	y=1.82×10⁴x+7.94×10²	0.9998	91.8, 103.9, 101.3	6.1, 2.6, 2.1	98.2, 102.5, 104.5	2.4, 1.9, 1.1
18	y=6.87×10⁴x-2.60×10³	0.9997	100.5, 104.4, 107.3	4.6, 1.9, 1.8	94.3, 98.2, 105.4	3.2, 3.1, 2.3
19	y=1.90×10⁴x-1.99×10³	0.9996	96.9, 105.5, 107.2	5.6, 3.1, 2.4	93.4, 99.0, 106.1	3.6, 1.7, 2.6
20	y=1.39×10⁴x-1.47×10³	0.9999	99.2, 100.1, 106.8	6.4, 3.4, 1.5	93.8, 91.5, 106.2	3.7, 3.1, 2.6
21	y=4.39×10⁴x+1.26×10⁴	0.9984	84.8, 107.6, 95.0	4.3, 0.9, 2.8	101.3, 103.4, 101.6	3.0, 2.6, 1.9
22	y=3.35×10⁴x+8.91×10³	0.9975	92.1, 107.1, 105.4	6.0, 4.0, 2.5	97.6, 102.6, 105.2	7.1, 3.8, 1.6
23	y=7.12×10⁴x+1.64×10⁴	0.9978	91.7, 109.1, 103.9	6.1, 3.7, 2.3	93.1, 105.8, 104.9	6.6, 3.9, 2.0
24	y=4.38×10⁴x+7.62×10³	0.9984	98.4, 109.4, 107.0	6.3, 4.2, 2.5	96.8, 102.1, 107.8	5.8, 2.2, 2.4
25	y=9.84×10³x-1.97×10³	0.9994	94.0, 107.3, 98.8	4.4, 3.7, 2.2	91.8, 102.6, 101.3	5.1, 2.8, 1.2
26	y=4.27×10⁴x-4.32×10³	0.9995	93.5, 96.6, 99.8	5.2, 1.8, 1.8	90.7, 88.9, 101.5	3.3, 2.8, 1.4
27	y=2.92×10⁴x+1.44×10³	0.9991	96.9, 106.6, 105.6	5.3, 2.0, 1.9	94.5, 100.7, 107.1	4.1, 2.7, 2.2
28	y=3.47×10⁴x+2.50×10³	0.9990	86.9, 108.2, 97.5	4.3, 2.1, 2.1	93.7, 102.1, 100.1	4.7, 2.8, 2.4
29	y=2.66×10⁴x+1.27×10⁴	0.9971	85.9, 107.6, 100.8	6.0, 3.8, 1.7	93.8, 108.0, 103.4	4.4, 2.7, 1.9
30	y=4.07×10⁴x+1.63×10⁴	0.9980	83.1, 108.2, 98.2	5.1, 2.2, 2.1	92.3, 104.0, 103.0	4.8, 2.6, 2.1
31	y=2.64×10⁴x+1.73×10⁴	0.9937	80.5, 110.9, 100.0	7.6, 3.4, 1.8	91.9, 109.2, 104.0	3.6, 2.4, 1.7
32	y=7.75×10³x+4.87×10³	0.9928	94.8, 98.0, 103.5	7.2, 4.9, 0.7	88.7, 109.3, 106.6	6.5, 2.6, 1.7
33	y=1.28×10⁴x-7.76×10²	0.9996	92.6, 103.3, 102.0	4.2, 2.4, 2.6	95.0, 104.2, 103.5	2.2, 2.1, 3.4
34	y=3.62×10⁴x+2.58×10³	0.9992	94.2, 107.7, 101.5	6.1, 2.4, 3.5	84.1, 102.6, 92.8	12.0, 2.9, 12.9
35	y=5.73×10⁴x+9.50×10³	0.9983	86.4, 109.6, 99.5	5.0, 2.2, 1.7	96.8, 107.2, 104.0	3.6, 2.3, 2.1
36	y=1.88×10⁴x-9.66×10²	0.9997	85.9, 105.4, 92.1	6.2, 4.0, 2.4	88.2, 105.3, 100.8	5.1, 3.6, 2.2
37	y=4.73×10⁴x+1.13×10⁴	0.9966	94.4, 111.1, 105.0	6.7, 2.2, 1.7	91.3, 103.9, 104.3	2.7, 1.4, 1.8
38	y=1.93×10⁴x+6.83×10²	0.9989	87.5, 106.0, 98.2	5.5, 1.7, 2.8	104.5, 104.5, 105.5	5.7, 2.6, 1.8
39	y=6.78×10⁴x-2.80×10³	0.9998	92.3, 102.0, 100.9	4.7, 1.9, 2.3	98.1, 98.3, 104.7	3.1, 2.5, 2.1
40	y=1.18×10⁵x+1.10×10⁴	0.9990	87.4, 109.8, 98.2	6.3, 2.1, 1.6	98.2, 105.1, 102.4	3.5, 1.6, 2.1
41	y=5.26×10⁴x+1.30×10⁴	0.9988	85.0, 109.6, 97.8	5.2, 2.2, 1.8	99.0, 106.8, 102.6	3.6, 2.1, 2.4
42	y=1.02×10⁴x+4.03×10³	0.9957	84.1, 109.4, 98.0	8.5, 3.9, 1.6	105.8, 101.9, 103.4	7.4, 6.0, 1.8
43	y=5.53×10⁴x+7.11×10³	0.9993	85.9, 107.5, 97.1	5.6, 2.4, 1.5	97.4, 108.7, 103.4	2.2, 2.8, 2.1
44	y=8.67×10⁴x+1.17×10³	0.9995	86.1, 107.0, 93.6	5.8, 2.2, 2.1	96.9, 107.0, 100.5	4.3, 2.9, 2.4
45	y=4.99×10⁴x+1.40×10⁴	0.9988	86.7, 105.1, 99.0	5.6, 2.8, 2.2	96.5, 106.9, 105.3	4.0, 3.3, 1.8
46	y=6.95×10⁴x+1.41×10⁴	0.9967	87.9, 102.9, 98.9	5.4, 2.8, 2.0	94.6, 105.0, 107.3	3.4, 3.6, 1.7
47	y=4.45×10⁴x-2.78×10³	0.9993	94.3, 108.6, 102.7	5.9, 2.4, 2.4	94.0, 102.4, 102.5	2.5, 1.2, 1.7
48	y=8.99×10³x+9.66×10²	0.9996	83.6, 109.1, 96.8	6.4, 4.0, 1.8	95.5, 104.2, 102.8	5.7, 3.4, 1.4
49	y=1.75×10⁴x+1.81×10³	0.9992	86.8, 105.9, 96.7	6.2, 2.3, 1.2	99.0, 105.8, 103.8	3.2, 5.6, 1.4
50	y=2.31×10⁴x+3.25×10³	0.9996	87.1, 106.5, 98.7	6.6, 1.5, 1.4	98.3, 107.0, 104.3	5.1, 3.0, 1.3
51	y=1.68×10⁴x-1.52×10³	0.9997	97.5, 106.8, 103.1	6.9, 3.7, 2.4	91.1, 102.3, 102.3	2.1, 2.8, 2.0
52	y=1.07×10⁴x+1.17×10³	0.9997	82.1, 104.0, 97.7	8.6, 1.7, 1.5	100.1, 98.4, 100.8	3.5, 4.3, 2.4
53	y=1.09×10⁴x-2.33×10²	0.9985	86.6, 105.3, 93.3	6.0, 2.2, 2.6	102.1, 104.6, 101.9	3.5, 3.4, 2.3
54	y=1.13×10⁴x+8.04×10²	0.9997	88.7, 105.2, 102.6	6.3, 2.6, 1.6	98.0, 99.1, 104.4	4.2, 4.0, 2.5
55	y=1.07×10⁵x-1.45×10³	0.9991	84.7, 107.1, 93.8	6.4, 1.5, 2.8	94.9, 107.8, 94.4	4.8, 2.3, 2.4
56	y=6.49×10⁴x+4.88×10³	0.9993	88.6, 107.6, 98.4	5.8, 3.6, 1.6	100.9, 101.2, 103.6	2.6, 3.3, 1.0
57	y=1.56×10⁵x+4.83×10⁴	0.9972	87.0, 109.7, 99.0	6.1, 2.2, 2.0	96.6, 108.1, 104.8	3.4, 1.4, 1.5
58	y=3.00×10⁴x+3.92×10³	0.9985	90.2, 108.4, 102.2	5.3, 2.6, 2.1	96.6, 103.3, 104.8	4.8, 4.3, 2.7
59	y=1.62×10⁴x-3.42×10²	0.9999	86.1, 105.6, 95.5	5.7, 2.6, 1.5	93.2, 105.8, 102.6	5.3, 1.8, 2.0
60	y=8.93×10³x+1.77×10³	0.9980	84.3, 108.4, 97.3	6.6, 4.8, 1.3	88.1, 108.2, 103.5	7.3, 4.4, 1.5
61	y=1.29×10⁵x+1.79×10⁴	0.9990	81.0, 104.6, 93.2	5.0, 2.7, 2.0	91.4, 106.8, 96.6	4.5, 1.4, 4.1
62	y=1.09×10⁵x-1.83×10³	0.9996	85.9, 109.2, 94.9	5.9, 3.6, 2.0	99.5, 106.8, 100.6	3.2, 3.0, 1.5
63	y=2.12×10⁴x-2.68×10²	0.9993	99.5, 110.5, 105.4	6.6, 2.3, 1.7	95.9, 108.7, 104.5	7.4, 3.1, 0.9
64	y=3.88×10⁴x+2.89×10³	0.9996	85.0, 106.9, 95.8	5.9, 2.9, 2.5	98.0, 103.8, 99.0	3.2, 3.5, 1.2
65	y=3.23×10⁴x-0.37×10²	0.9993	84.7, 107.8, 95.1	5.0, 2.2, 2.7	91.7, 101.2, 98.8	5.2, 2.3, 1.2
66	y=2.73×10⁴x+3.01×10³	0.9990	97.5, 108.6, 107.2	7.6, 2.3, 1.8	94.7, 106.6, 105.0	2.7, 2.6, 1.8
67	y=1.79×10⁴x-1.80×10³	0.9992	82.6, 107.4, 91.4	8.8, 3.0, 1.7	97.5, 104.5, 101.9	6.1, 3.4, 3.2
68	y=4.98×10⁴x+1.08×10⁴	0.9992	82.7, 108.8, 97.0	8.6, 2.9, 1.4	97.0, 104.0, 104.1	3.8, 3.6, 2.8
69	y=5.12×10⁴x+9.36×10³	0.9984	85.4, 110.6, 98.1	8.4, 4.0, 3.0	98.0, 111.4, 105.2	7.2, 3.0, 1.4
70	y=9.26×10⁴x+2.56×10⁴	0.9983	79.7, 106.4, 94.3	7.2, 2.5, 1.2	98.1, 106.2, 102.4	5.8, 3.8, 2.2
71	y=2.87×10⁴x-3.48×10³	0.9998	91.7, 104.4, 99.3	6.2, 3.1, 2.2	100.3, 107.3, 102.7	6.3, 4.5, 1.0
72	y=4.68×10⁴x+8.92×10³	0.9981	86.6, 108.3, 98.5	4.7, 2.6, 1.9	96.1, 107.7, 100.1	2.8, 3.5, 1.5
73	y=4.24×10⁴x+5.47×10³	0.9979	89.1, 111.5, 98.6	6.1, 0.9, 2.5	97.1, 108.5, 104.0	2.7, 2.6, 1.6
74	y=8.01×10⁴x-3.76×10²	0.9995	88.9, 106.7, 96.7	6.0, 1.5, 1.5	98.0, 106.2, 100.3	3.2, 1.6, 1.1
75	y=5.82×10⁴x+4.28×10³	0.9995	80.3, 105.9, 92.9	6.3, 4.9, 1.3	96.0, 107.2, 97.8	4.3, 1.9, 1.8
76	y=5.12×10⁴x+4.08×10³	0.9990	86.8, 106.8, 98.1	5.5, 2.0, 1.2	98.3, 101.9, 102.8	4.3, 2.7, 2.2
77	y=3.08×10⁴x-3.61×10²	0.9987	86.7, 105.8, 94.9	5.7, 2.3, 2.5	104.4, 106.1, 99.5	5.0, 3.9, 2.7
78	y=3.49×10⁴x-2.10×10³	0.9995	84.5, 109.1, 95.2	6.3, 1.3, 2.1	102.0, 105.6, 99.5	6.0, 2.8, 1.6
79	y=2.68×10⁵x+1.67×10³	0.9993	87.6, 107.3, 97.7	6.2, 3.5, 2.4	96.9, 104.3, 101.8	4.2, 2.7, 1.7
80	y=2.15×10⁴x+2.52×10³	0.9995	81.1, 108.7, 91.9	6.4, 4.5, 1.5	96.6, 106.0, 97.7	3.6, 1.9, 2.3
81	y=6.34×10⁴x+2.53×10⁴	0.9972	79.9, 110.3, 96.8	7.5, 2.0, 2.1	95.8, 110.0, 99.1	5.3, 3.2, 2.1
82	y=1.83×10⁴x-2.41×10²	0.9995	83.1, 107.1, 95.5	7.1, 1.9, 2.7	95.3, 102.2, 93.9	4.4, 5.7, 1.3
83	y=8.21×10⁴x+2.05×10³	0.9989	83.2, 103.8, 92.7	6.0, 5.6, 1.4	93.8, 102.7, 98.8	5.6, 3.7, 1.5
84	y=6.38×10⁴x-4.05×10²	0.9993	86.2, 108.9, 96.4	6.3, 4.8, 3.5	98.7, 106.5, 99.3	4.4, 3.1, 1.7
85	y=2.97×10⁴x+4.26×10³	0.9992	83.6, 107.8, 96.0	6.5, 2.8, 2.2	98.4, 107.6, 102.3	4.6, 2.1, 1.5
86	y=1.58×10⁴x+4.51×10³	0.9980	87.5, 113.8, 99.0	5.8, 1.3, 1.0	92.1, 112.1, 101.0	3.1, 3.4, 3.1
87	y=1.45×10⁴x+6.08×10³	0.9982	80.0, 112.0, 97.9	9.4, 2.7, 2.2	93.7, 107.1, 105.9	5.6, 5.1, 1.7
88	y=3.36×10⁴x-0.79×10²	0.9996	83.9, 107.1, 94.7	7.4, 3.8, 1.9	104.2, 109.5, 99.3	3.8, 3.0, 3.2
89	y=7.14×10⁴x+2.47×10²	0.9988	90.0, 108.8, 96.4	5.4, 2.7, 1.7	99.0, 107.0, 101.9	6.6, 2.5, 0.7
90	y=6.94×10⁴x+1.85×10⁴	0.9983	83.6, 101.6, 95.6	7.3, 1.7, 2.1	84.9, 94.3, 94.6	5.1, 2.4, 2.4
91	y=4.77×10⁴x+6.96×10³	0.9988	84.9, 109.2, 96.7	7.2, 1.6, 1.8	97.4, 106.8, 103.6	4.4, 3.3, 1.2
92	y=6.10×10⁴x+2.75×10⁴	0.9955	81.3, 114.4, 98.3	8.4, 2.7, 2.3	97.6, 111.7, 103.4	5.1, 3.2, 1.2
93	y=2.81×10⁴x+3.21×10³	0.9993	81.3, 107.2, 96.7	7.8, 5.4, 1.9	98.1, 104.7, 98.5	2.6, 2.2, 0.9
94	y=3.83×10⁴x+8.97×10³	0.9989	81.1, 100.2, 95.2	5.1, 0.9, 2.2	100.0, 107.9, 102.8	2.5, 2.0, 1.9
95	y=7.20×10⁴x+1.10×10⁴	0.9994	81.1, 105.3, 97.1	6.3, 2.1, 2.8	97.1, 105.2, 99.6	5.3, 2.0, 1.6
96	y=1.95×10⁴x+5.24×10³	0.9984	79.6, 106.1, 93.7	8.4, 2.4, 2.0	94.3, 107.9, 103.2	7.2, 3.3, 1.2
97	y=4.78×10⁴x+1.76×10⁴	0.9970	79.7, 110.4, 96.5	8.5, 3.4, 1.7	96.0, 111.6, 102.6	1.5, 0.9, 1.2
98	y=8.82×10⁴x+9.81×10³	0.9989	82.5, 105.4, 96.3	7.8, 2.1, 2.2	97.6, 105.2, 99.6	4.1, 2.3, 2.1
99	y=1.15×10⁵x+9.19×10³	0.9996	82.5, 108.6, 94.7	6.5, 2.9, 1.8	94.6, 105.0, 96.9	3.2, 1.7, 0.9
100	y=1.65×10⁵x+3.65×10⁴	0.9998	81.6, 105.9, 98.4	9.2, 2.2, 3.6	88.1, 100.0, 80.9	2.5, 1.2, 1.3